FI58047B - FOERFARANDE FOER FRAMSTAELLNING AV EN STABIL KONCENTRERAD KRAFTIGT SMAKANDE AROMATISK PRODUCT - Google Patents

Description

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National Board of Patents and Registration (44) Date of issue and date of issue: 'Q no Rf)

Patanfe · och registerstyrelsen 'Ansakin utitgd och utUkrifwn pubiinrad. uo. ou (32) (33) (31) Captured «Bugird prlorttet (71) The Procter & Gamble Company, 301 East Sixth Street, Cincinnati,

Ohio 45202, USA (72) Rudolf Gottfried Karl Strobel, Cincinnati, Ohio, USA (74) Oy Kolster Ab (54) Method for producing a stable, concentrated, strong-tasting, aromatic product - Förfarande för framställning av en stabil , concentrates, kraftigt smakande, aromatic product

The present invention relates to a process for the preparation of a stable, concentrated, strong-tasting, aromatic product from a flavor-containing substrate, said substrate being maintained at a temperature of about 0-60 ° C and extracted by slowly feeding moist steam to the substrate-containing column in a manner that prevents flooding while maintaining the column at an absolute pressure of about 0.1-200 mmHg.

Many food products, and especially those made from extracts for brewery products, are known to contain small amounts of both flavors and aromas. These flavors and aromas give the fresh product a sensual balance of taste and aroma. However, it is very common for these types of foods to develop a rapidly rancid aroma when exposed to atmospheric conditions. This rapidly developing rancidity in aromiesans often significantly degrades the taste of any beverage isolated and prepared from food product extracts. In addition, compounds that promote aroma rancidity often act as catalysts for the rapid development of rancidity in the spice components of beverages. Therefore, while certain highly volatile essences containing flavoring agents are highly desirable for providing a pleasant first sensory impression, they are less desirable over time because they promote the rapid development of both aroma and taste saturation.

Some well-known food products, such as coffee, tea, and certain fruits, such as oranges, grapefruits, strawberries, and cherries, are often prepared by extraction into concentrated extracts that can either be dried or diluted to make soft drinks. It is typical that during the extraction, the aforementioned delicate balance of flavor-containing essences and spice-containing essences is disturbed when exposed to the thermal and pressure conditions required for an efficient extraction process. Thus, the final beverage extract or dried material contains flavors and aromas in a completely different proportion than the original food product. For many years, those skilled in the art have approached this problem by trying to separate the aroma-containing essences from the natural food product before extraction, and to add the aroma-containing essences again after the extraction process. That is, the aroma essences are removed, the remaining portion is brought to the required temperature and pressure conditions suitable for high extraction yields, and then the aroma-containing essences are added back. Although this method has achieved widespread success, especially in the manufacture of coffee and tea-based products, it has certain inherent disadvantages. First, aroma-containing essences, when added back to the recovered extract, are often subjected to conditions during drying which cause a substantial deterioration in the taste and aroma they produce. Second, the extract remaining after removal of the aroma-containing essences contains many natural face-containing essences that deteriorate significantly and change, creating foreign flavors during the high pressure and temperature conditions required to achieve the most efficient extraction.

The process according to the invention is characterized in that the flavor concentrate residue is first recovered from the extract by condensation at a temperature of about -80 ° C to 200200 ° C before the liquid fraction separates from the column, the flavor concentrate is removed and, if desired, mixed , and that a separate flavor and concentrate concentrate which concentrates in a temperature range of about -80 to -200 ° C is then collected, which separate flavor and concentrate concentrate, if desired, is fractionated into a flavor concentrate which is collected by a cold trap at a temperature of about -80 ° C. , and a second flavor concentrate collected by a second cold trap at a temperature of about -200 ° C.

The liquid flavor concentrate is particularly suitable for dilution to form soft drinks. The flavor concentrate can be added back to the dried extract to provide flavor addition. Alternatively, the aroma and flavor concentrates can be recovered in a manner that prevents the deleterious effects between them, mix them with a solution of suitable solids, and freeze-dry the mixture to give a dry product with a high taste and face content.

The process is particularly suitable for providing a coffee flavor concentrate which is substantially free of highly volatile aromatic compounds which rapidly develop aging after exposure to ambient light and heat conditions and therefore give a foreign taste and aroma to the beverage, and for the production of stable, dry products with taste.

The method according to the invention is unique not only in terms of the result obtained but also in terms of its operating principle. The method makes it possible to prepare both flavor / aroma concentrates and dry products with stable taste and aroma content. The principle of operation is physicochemically complex because the process involves steam distillation (both wet and dry), desorption, conventional extraction, diffusion, dissolution as well as re-adsorption (chromatography). In this sense, the process is uniquely different and distinguishable from prior art processes for making coffee in which a flavored frozen product is condensed and subsequently added back to either the instant coffee extract, which is then concentrated and dried, or directly to the dried extract (see Lemonnier, U.S. Patent 2,680,687, which describes the dry distillation of coffee and the condensation of aroma essences at -180 ° C, Kline, U.S. Patent 3 k06 OTh-, which describes the separation of aroma essence fractions by distillation and concentration from roasted and ground coffee using vacuum conditions and temperatures not exceeding Ul ° C and Mook, U.S. Patent 3,035,922, which describes vacuum distillation of wet coffee powders at temperatures of 25 to 50 ° C and condensation of flavoring agents at temperatures of 0 to 80 ° C). These prior art methods, particularly applied to coffee, can be readily distinguished from the process of the invention in that none of these patents describe the essential separation of flavor essences from flavors, so that a liquid flavor concentrate and a flavor concentrate are obtained simultaneously; moreover, significantly different manufacturing conditions have been used in the past.

The method according to the invention can process not only roasted and ground coffee, but also many other nutrients, such as fruits, berries and vegetables, even potatoes.

The following describes coffee processing in more detail.

Roasted and ground coffee is loaded into a substrate zone, preferably an extraction column. In the preparation of separate flavor and aroma concentrates, "extraction" is carried out with cold, moist steam and the "extract" is separated into at least two parts, the first part being flavor concentrate and consisting of compounds freezing at or above -20 to -80 ° C, and the second part being an aroma concentrate consisting of compounds that freeze at a lower temperature than the first part. "Extraction" is performed under reduced pressure as shown below. It is recommended that before starting the process of the invention, the system be purged of oxygen by purging the entire system with an inert gas. This purging of the system with an inert gas before starting the extraction is performed to remove oxygen from the system, as the presence of oxygen in the system promotes the rapid development of degraded taste and aroma.

Prior to the treatment according to the present invention, the substance to be treated, such as coffee, can be frozen, for example, with the aid of liquid nitrogen, in order to ensure the development of the best taste and facial concentrates. It is recommended to do this freezing before possible comminution, in order to reduce the formation of your free radicals during the comminution step, as these can spoil the flavor and flavor concentrates that can be separated later. The formation of free radicals can occur during typical mechanical stressing effects, such as grinding, flaking or other comminution processes, unless the substance is first frozen.

According to the present invention, the extraction is carried out with moist steam which is passed either in impulses or slowly and continuously through a substance to be treated, such as roasted and ground coffee. It is important to note that moist steam must be fed to the extraction column slowly, i. as a pulsed or slow continuous addition, otherwise the flavoring and flavoring ingredients will not be sufficiently separated; in addition, it has been found that only in this way a liquid taste concentrate with a satisfactory taste is obtained. It is recommended, though not necessary, for the color-forming agents and color precursors to be passed through the system that the method be performed downstream. However, as will be explained below, upward supply of moist steam is also possible.

Of course, the process can be carried out, if desired, by varying the pulsed and continuous feed, as long as the conditions are arranged so that the steam is moist and its feed is slow. As mentioned, if the whole column is filled with water, no satisfactory separation into liquid flavor concentrate and aram concentrate occurs. Besides, if the column is completely wetted in the early stages of the process, it becomes a mere cold extraction process, and a conventional extraction liquid is obtained, and not a liquid flavor concentrate, which is a unique stability.

In normal practice, moist steam as such is not fed directly to the column, but hot water is preferred, so that the water • evaporates rapidly from the vacuum conditions used in the column, producing cold steam. Since the substance to be treated is usually cooled before it is placed in the extraction column, some of the steam condenses rapidly on the surface of the substance.

According to the recommended method, hot water close to 100 ° C is fed to the upper end of the zone containing roasted and ground coffee. For the reasons described above, the water evaporates rapidly to produce cold (about 20 ° C), moist steam. The first impulse should comprise such a small amount of steam that only the beginning of the column is wetted, usually about one-tenth or one-eighth of the column. Once the first steam boost is fed, it quickly comes into contact with roasted and ground coffee, which is usually at a lower temperature than the steam. Upon immediate contact with steam, the most volatile flavors are desorbed from the substrate and by gravity and vacuum and, as explained in more detail below, by continuously flushing down with an inert gas, when used, they pass down through the column. It is these most volatile aromatic substances that most often contribute to the rapid rotting of the flavor and aroma concentrates and it is therefore desirable that they be removed immediately at the beginning of the process.

As soon as the first impulse of steam hits the nutrient substrate and the most volatile substances are desorbed as described above, the steam condenses on the surface of the coffee particles and begins to be absorbed into the particles. This in turn causes more gas desorption and similarly these aromatic essences are transported down to the column. Eventually, the water saturates the outer parts of the particles and due to the vacuum conditions, the water begins to evaporate from the outer surface of the particle and form cold steam. In this way, the water-soluble flavors migrate to the outer surface of the particles, from where they can be removed by the next impulse of moist steam. The substrate downstream of the interface is preferably kept at a sufficiently high temperature to avoid re-condensation of these removed substances.

After the first wet steam impulse, a clear interface can be observed between the dry coffee particles that have not been exposed to the cold moist steam and the particles that have been exposed to the cold moist steam. This interface includes a dark-toned zone due to the presence of color-containing substances. With each subsequent push, the zone gradually moves down through the column and the whole process involves cold vapor desorption of highly volatile substances, water absorption and further desorption of slightly less volatiles, evaporation of water towards the surface of the particles and cold steam distillation to reflux the concentrate.

In impulses, the effect of the cold moist steam is allowed to continue in this way until the "burst" of the zone. As used herein, an outbreak is defined as the time at which the first flavor concentrate zone has reached the bottom of the column.

Separation and recovery of flavor and aroma concentrates is preferably performed using two "cold traps" in series (one at about -20 to -76 ° C and the other at about -200 ° C), as this allows recovery of the flavor concentrate as a stable frozen.

Before the outbreak of the zone, almost colorless frozen food accumulates in the first trap. The colorless frozen substance consists largely of water-soluble alkaline and 6 58047 neutral aromatic substances as well as aromatic phenolic and / or acidic substances. This first frozen can either be discarded or, if desired, subjected to the process disclosed in U.S. Patent 3,579,300. After being subjected to the process of the above-mentioned patent, the colorless frozen product is divided into acidic flavored fractions which can be added back to conventional spray-dried instant coffees to improve their aroma and taste.

Once the outbreak of the zone has occurred, the liquid flavor concentrate accumulates in the first trap. This liquid flavor concentrate is unique and differs from conventional extract concentrates in many respects. First, the liquid flavor concentrate is very stable; this is because highly unstable volatile aromatic essences have been removed from it. Second, the liquid flavor concentrate is prepared using very low temperatures compared to conventional extraction temperatures and therefore contains various flavor ingredients. Third, the liquid flavor concentrate can be diluted without further processing to obtain a tasty beverage of excellent quality and taste stability.

Once the zone burst has occurred, vacuum conditions can be maintained in the column until the tops of the charged roasted and ground coffee zone are again substantially dry and the pulsed supply of moist steam can continue as described above. The steam pulses are continued until the gradually downward zone of the flavor concentrate is substantially free of color-containing substances. At this point, the zone, in terms of roasted and ground coffee, changes to light brown in color and t% ä indicates that most of the color-containing substances, color-containing substance precursors and flavors have been removed. At this point, the column is emptied and a new batch of roasted and ground coffee is inserted and the method is repeated.

At the same time as the liquid flavor concentrate is collected in the first trap, the highly volatile substances pass through this first trap without condensing and pass into the second trap maintained at the temperatures of the liquid nitrogen. In this second trap, the aromatic concentrate is collected frozen.

The process of this invention is preferably carried out by passing an inert gas through the system of about 0.2 to 25 l / min and more preferably about 2.5 l / min per m of cross section of the column (perpendicular to the flow). The inert gas may be nitrogen, argon, helium, freon, etc. Preferably, the inert gas is a combination of nitrogen and carbon dioxide in a ratio of about 1: 9 ~ 9: 1, which surprisingly provides a taste-enhancing effect on the flavor concentrate to be separated later. This rinsing feature helps to transport flavoring and aromatic substances through the column. After purging the column with this inert gas containing at least some carbon dioxide, the carbon dioxide condenses with the aroma concentrate in the second trap. In this case, carbon dioxide or another inert gas having a freezing point between the temperatures of the KaMe trap solidifies with the aroma-containing substances in the form of frozen aroma-CO 2 tritium in another trap. This is highly desirable because carbon dioxide acts as a diluent and protective medium for highly reactive face-containing substances by separating portions of the flavor concentrate. This is advantageous because it makes it possible to maintain the arcmi concentrate in a relatively stable state that prevents an internal chemical reaction between different parts of the concentrate. Once such an interaction has begun (which can occur even under the influence of light), it continues autocatalytically throughout the aroma concentrate and rapidly develops rancidity.

The resulting arami concentrate frozen (with or without CO 2) can be removed from the second trap and covered with coffee oil and placed under ambient conditions. All the carbon dioxide is easily sublimated as the temperature rises slowly, leaving a highly aromatized coffee oil that can be used to be added back to conventionally prepared dry instant coffees. Alternatively, the solid aroma-CC 2 frozen can be mixed with frozen coffee oil, ground to a fine powder and brought to ambient conditions to give an improved aroma coffee oil.

Another unique feature of the process of this invention is that the taste of the liquid flavor concentrate can be precisely controlled to obtain a concentrate that tastes either very mild, filter coffee-like, or coarse and strong, which is characteristic of very strong beverages. This is accomplished by carefully adjusting the grinding size of the nutrient substrate contained in the column as well as the temperature inside the column.

In particular, it has been found that liquid flavor concentrates with very mild taste properties are obtained when the column is maintained at 0-60 ° C (substrate temperature rapidly approaches the temperature at which the column walls are maintained) and the nutrient substrate, in this case roasted and ground coffee, is ground very finely. As used herein, the phrase "very fine grinding size" is understood to mean a grinding size of less than 0.85 nm. If, on the other hand, the aim is to develop a unique filter coffee-like taste, it has been found that the grinding size of roasted and ground coffee in the column should be medium ground (0.30-2.3 mm) and the temperature of roasted and ground coffee in the column should be adjusted to 30- 60 ° C. Furthermore, if it is intended to produce a very strong or even bitter-tasting liquid flavor concentrate, the grinding size should be very coarse (greater than 2.8 mm) and the temperature of the roasted and ground coffee incorporated in the column should be between 60-95 ° C. If a mixture of all these taste effects is desired, a grinding gradient starting from coarser particles at the top of the column, continuing with medium grinding in the middle and ending with fine grinding near the bottom can be used, provided that the process is carried out in the downstream direction. In addition, the grinding gradient β 58047 tit helps to eliminate the problems caused by the unevenness of the liquid flow.

Yet another unique feature of the liquid flavor concentrate prepared by the process of this invention is that the yield of the beverage made from the liquid flavor concentrate is equal to and in most cases higher than the yield obtained from either roasted and ground coffee extraction or conventional instant coffee. 100 g of roasted and ground filter coffee typically gives 15 cups (1 cup corresponds to 150 ml) of a satisfactory beverage ^ instant coffee made from 100 g of roasted and ground coffee normally gives 20 cups of beverage. The process of this invention provides a liquid flavor concentrate that can be diluted to at least 20 cups per 100 g and normally 25 to 30 cups and in some cases up to 35 cups per 100 g. In addition to the beverage yield, the method naturally also provides a facial concentrate.

It is essential for the process of the present invention that the vacuum pressure at the interface between the moist steam zone and the dry roasted and ground coffee is 0.1-200 mmHg and preferably 0.1-30 nmHg. When absolute pressures higher than 200 nmHg are used, cold moist steam is not sufficient to obtain a liquid flavor concentrate with satisfactory properties. The minimum pressure is given here only as a practical lower limit.

The amount of dilution of the liquid flavor concentrate required to make a satisfactory beverage will, of course, depend on the precise conditions used to keep the process running and how long the process is maintained. The part of the flavor concentrate zone that is collected in the first traps immediately after the outbreak of the zone is the most concentrated and the part that is collected after the process has been continuously running for some time is the dilute.

With respect to the method of the present invention, it should be further noted that although the method specifically disclosed herein is a batch process, a semi-continuous and continuous process may also be used. Furthermore, although the preferred downward impulse method for wet steam desorption is specifically described herein, it is possible to use upward impulse desorption, downward slow, continuous desorption, upward slow, continuous desorption, and horizontal and oblique flow desorption processes. When using upward desorption, the vacuum must, of course, be drawn primarily upwards. In addition, it is recommended to use a sieve or other retaining member at the top of the column to facilitate recovery of the flavor concentrate.

As mentioned above, when a continuous supply of moist steam takes place as opposed to a pulsed supply, it is essential that the supply is slow and continuous. For the reasons mentioned above, it is not desirable for the pulse method for the column to be flooded before it bursts, and if a rapid, continuous supply of steam 58047 9 is used, flooding will occur. As a general guideline, when using a slow, continuous supply of moist steam, the amount of steam added during the entire period before the onset should not be greater than in the impulse process.

The zone containing the substrate, in most cases a column, may be of any suitable geometric shape, but is preferably cylindrical and for best results is about 2.5 cm to 2 m in length and preferably 30 cm to 1.2 m in length. m usually need to use coarser grinds, which results in lower yields and less recommended crude flavors. When using columns longer than 1.2 m, it is recommended to apply a pressure at the steam supply point of the column that is higher than that required at the interface to push the interface between the moist steam and the dry beans downwards in the column. In this variation, there is still a vacuum of about 0.1-200 torr at the interface. Care must be taken to use sufficiently high steam or water supply temperatures to prevent the formation of a complete water barrier. Such a "pressure" application in steam supply can also be used to reduce the extraction time (i.e. to increase the migration rate of the interface).

Many variations on the use of liquid flavor concentrate are quite obvious. If desired, it can be packaged in a suitable dispenser and sold as a liquid concentrate, it can be gently freeze-dried, it can be lyophilized and then freeze-dried and spray-dried, it can be used as a beverage flavor concentrate, ice cream manufacturing and hot and cold plots. With respect to still a dispenser use, one suitable use that utilizes both flavor concentrate and flavor concentrate is to use a dual dispenser that simultaneously distributes flavor concentrate and flavor concentrate to the flavor concentrate stream. This produces an aromatic drink and the cold aroma of fresh ground coffee.

The following examples are provided to illustrate the method of the present invention insofar as the invention is applied to various nutrient substrates, in particular coffee, tea, strawberries, oranges and peanuts, for the preparation of separate flavor and aroma concentrates therefrom.

Example 1

A coffee column 12.7 cm wide and 15.2 cm long was joined together by two successive sealing traps. The first trap was kept at 7676 ° C with dry ice. The second trap was maintained at -195.8 ° C with liquid nitrogen. A vacuum pump was connected to the system to allow the use of vacuum pressures during the process.

900 g of roasted coffee beans were frozen in liquid nitrogen and ground to a fine grinding size, i.e. less than 0.25 mm. To purge the system of oxygen, ίο 5 80 4 7 Ten grams of solid carbon dioxide was placed on top of the beans and allowed to sublime and pass through the system to displace oxygen. The roasted and ground coffee was placed on the column in this and the following examples, unless otherwise stated, from 90 to 100 ° C, water was fed in to produce moist steam, which was driven in bursts down the column zone under the conditions shown:

table 1

Time (min) Temperature (° C) [vacuum (torr) Water addition (ml) 0 - 3 ^ UOO (total) 5 50 0.6j 10 k2 0.5 100 15 60 0.5 1 + 00 25 50 0.5 1 + 00 1 + 0 1 + 5 0.5 200 55 1 + 5 0.5 300 60 1 + 7 0.5 200

Cold moist steam was passed down through the column in bursts and fed approximately equal amounts at approximately two minute intervals. The amounts listed in the table represent the total amount of steam (water) entered between successive time points at which the results were recorded. The column was maintained at the temperatures indicated above by means of a water jacket. After the steam was passed for 10 minutes, a dark, almost black zone of matter was clearly visible in the upper parts of the column. During the run, this zone continuously moved down through the column until it erupted. Prior to eruption, a colorless frozen was collected from the first trap and removed. The liquid flavor concentrate was then collected in the first trap and by the time the run was stopped (near final catch) a total of 775 ml of this dark, almost black liquid flavor concentrate had been collected »This concentrate had a very pleasant coffee aroma and when 15 ml of this liquid concentrate was added in hot tap water (150 ml) gave a beverage with a pleasant coffee taste and aroma. The taste was found to be typical of mild, high-grown film grades. The liquid flavor concentrate was allowed to stand at ambient conditions for 5 and 15 days and, when examined, had a consistently pleasant taste and aroma and was obtained by diluting an excellent mild and somewhat filter-type beverage.

At the same time as the liquid concentrate was collected as described above, a solidified aroma frozen consisting of coffee aroma and carbon dioxide solidified into an aroma CCl 2 matrix accumulated in another trap maintained at liquid nitrogen temperatures. This aroma-CO 2 matrix was placed in ho ml of pressed film oil and allowed to equilibrate until all CC 2 was U 58047 sublimed. The coffee oil was found to have an excellent coffee-like aroma and when added to spray-dried instant coffee in an amount of 0.2% by weight in the conventional manner, it significantly improved the aroma of the product.

Results similar to those shown in this example are obtained when repeated using a slow, continuous addition of moist steam instead of a single pulse. The continuous process used the same amount of steam as used in the pulse increment shown here.

Example 2 The procedure described in Example 1 above was used. The total amount of roasted and ground coffee ground to a grinding size of 0.30-0.60 mm was 1200 g. The entire system was purged of oxygen by placing a small amount of dry ice in the system before starting the process. The process was run using the conditions shown in the following table:

Table II

Time (min) Temperature (° C) Vacuum (torr) Addition of water (ml) 0 55 0,5 600 5 55 0,5 ") UOO (total)

10 55 0.5J

15 55 0.5 500 30 55 0.5 700 35 55 0.5 800 U5 55 0.5 500

Prior to the onset of the zone, a colorless frozen appeared in the first trap and was removed. Thereafter, while the downward impulse supply of steam was continued as shown in the table, an inch black zone was observed in the column, which gradually moved downward at the interface of moist steam and dry beans. The total amount of liquid flavor concentrate collected in the first trap was 1900 ml. The trap was kept at 7676 ° C in a bath of dry ice and acetone. The second trap was cooled to liquid nitrogen temperatures and at the same time as the liquid flavor concentrates were collected, the aroma and carbon dioxide frozen solidified in this second trap.

The highly volatile aroma portion collected in the second trap was added to the liquid flavor concentrate collected in the first trap, and while the intensity of the original aroma clearly increased, it was found that within 10 minutes the flavor concentrate tasted and developed rapidly signs of spoilage and rancidity. Taste changes were observed to persist over time. Therefore, it was concluded that the mere addition of highly volatile flavors from the solidified Arani-CO 2 frozen to the liquid flavor concentrate was not desirable because the highly volatile compounds rapidly decomposed and then acted as catalysts, rapidly degrading the liquid flavor concentrate.

Example 3 Using the procedure set forth in Example 1, 1 kg of frozen strawberries were subjected to the process of this invention. Before starting the process, 20 g of powdered carbon dioxide was added to the system to purge it of oxygen. The process was performed using the following conditions.

Table III

_Time (min) _Temperature (° C) _Vacuum (torr) _Water addition (ml) 0 0 0.2? 100 (total)

10 22 0.2J

15 1 + 0 0.2 300 35 23 0.2 300 50 25 0.2 100 60 25 0.2 200 70 35 0.2 200

Prior to starting the process, the frozen strawberries were ground to a grinding size of <3 nm.

At this point, when the steam was fed downwards as described above, the colored zone, which gradually moved downwards through the column at the interface of moist steam and "dry" strawberries, was found to be deep carmine in color. The aroma-COg matrix collected in the liquid nitrogen trap was found to contain a very pleasant but not particularly strong strawberry aroma. The liquid concentrate collected after onset in the first trap kept at 7676 ° C in a bath of dry ice and acetone was found to have a very strong strawberry flavor and a mild strawberry aroma. The color of the zone continuously deteriorated after the onset and when the process was stopped (70 min), the color of the zone was no longer very pink.

The liquid flavor concentrate was found to be stable on storage and did not develop any rancid odors. In addition, the liquid concentrate was found to be obtained by dilution using 20 ml of concentrate and 80 ml of water, a very pleasant strawberry-flavored beverage.

Example U

Using the procedure described in Example 1, peeled, frozen oranges, frozen in liquid nitrogen and finally ground to a size of ζ 3 mm, were placed on the column. 25 g of carbon dioxide was placed in the system and allowed to sublime to purge the system of oxygen. During the process of this invention, the system was continuously purged with downward carbon dioxide. The process was run under the following conditions: 13,58047

Table IV

Time (min) Temperature (° C) short (torr) Water addition (ml) 0 25 0.3) 300 (total) 10 13 0.3) 30 18 0.3 100 60 19 0.3 100 90 30 0.3 100 1 + 00 ml of liquid digestate concentrate was collected after the onset of the first trap. The zone that moved continuously downward through the column during the impulses of moist steam was found to be a bright, very intense orange in color. When the process was stopped (90 min), the substrate remaining on the column was found to be only very slightly orange in color. The liquid flavor concentrate had a very pleasant orange aroma and when diluted to 150 ml by adding 75 ml of water to 75 ml of the liquid flavor concentrate, an excellent orange-flavored beverage was obtained which did not develop any noticeable fading or wilting for 5 hours. conditions.

The liquid nitrogen trap contained a very pleasant but not very strong orange flavor COg matrix.

Example 5 310 g of unsalted peanuts were frozen in liquid nitrogen and crushed to an estimated grain size of 0.85 mn. Peanuts were treated as described in Example 1 using the following conditions:

Table V

Time (min) temperature (° C) Vacuum (torr) Water addition (ml) 0 22 0, θ) 200 (total) 5 U0 0,1 + 3 10 30 0,1+ 300 25 30 0,1+ 200

As in the case of the above examples, the wall of the column was maintained at the temperatures of the region described above with a cold water jacket surrounding the column.

1 + 75 ml of liquid flavor concentrate was collected in the first trap. The zone that moved continuously downward through the column as cold moist steam pulses downward was dark brown in color. The liquid flavor concentrate collected after the outbreak was found to have a very pleasant peanut odor and was found to be suitable for improving the taste and aroma of dry peanuts by spraying it on them in small amounts. The aroma matrix collected in the second trap maintained at liquid nitrogen temperatures was found to have a very strong peanut aroma.

m 58047

It was found desirable to add liquid peanut flavor concentrate to foods where the peanut flavor is desirable »e.g., cake powders, mixed bread powders, etc. When the flavor CO

Example 6 An apparatus similar to that used in Example 1 was used. However, since an upward impulse supply of steam was used in this example, successive sealing traps communicated with the top of the column and the column was continuously flushed from the bottom upwards with nitrogen gas. The vacuum was drawn from the top of the column. Near the top of the column, a perforated Plexi glass plate was placed on top of the nutrient substrate layer to match the diameter of the column.

2 kg of roasted coffee beans were frozen in liquid nitrogen and ground to a grain size of less than 0.85 mm. The roasted and ground coffee was placed on the column and moist steam was fed in bursts upwards through the column under the following conditions:

Table VI

Time (min) Temperature (° C) Vacuum (torr) Addition of water (ml) 0 70 0.2 ^ 3250 (total)

65 75 0.3J

125 75 0.3 1550 130 78 0.3 600 26Ο 78 0.3 36ΟΟ

Cold, moist steam was passed up through the column in bursts as shown in the table above with the additions described in Example 1. The column was maintained at the temperatures indicated above by means of a water jacket. As the steam bursts continued upward as shown in the table, a dark black zone was observed in the column that gradually moved upward at the interface between moist steam and dry beans. After the onset of the zone, 1650 ml of liquid flavor concentrate was collected in the first trap. The trap was kept at -76 ° C in a bath of dry ice and acetone. The second trap was cooled to liquid nitrogen temperatures and while the liquid flavor concentrate was collected, the arami concentrate solidified into the second trap.

Thereafter, the liquid spice concentrate was used to prepare coffee beverage samples that were almost impossible to separate from the freshly filtered coffee. The procedure used to prepare the beverage was similar to that shown in Example 1.

15 58047

Example 7

The procedure described in Example 1 was repeated using 906 g of a mixture of orange and black tea as a nutrient substrate. The tea was placed on the column and moist steam was fed in bursts down through the column under the following conditions:

Table VII

Time (min) Temperature (° C) Vacuum (torr) Addition of water (ml) 0 63 0, l) 6 59 0, lr 800 (total) 22 60 0, l) 52 60 0,1 1000 8b 60 0,1 1000 ll + o 60 0.1 800 210 60 0.1 1800 235 60 0.1 1800 260

After 3 minutes of steam, a clear emotional zone of matter could be observed in the upper part of the column. The zone moved continuously downward through the column at the interface of dry tea and moist steam. Prior to onset, the colorless frozen was collected in the first trap and removed. A total of 1 + 955 ml of liquid flavor concentrate was collected after the first trap. The flavor concentration11a had a very pleasant aroma and when diluted, a tea beverage of excellent quality was obtained. The flavor concentrate was freeze-dried to give 275 g of solids, i.e. a 30% yield.

In addition to the dry product prepared by drying (e.g., freeze-drying) the flavor concentrate, a stable, dry product of a unique nature can be prepared based on the "extraction" process described above using the variation now described. highly volatile ingredients which tend to react and give the product an undesirable character if left in a liquid state for more than about 30 minutes.To prevent the undesired interaction described here, flavorings may be trapped in one or more low temperature traps or added to a coffee oil carrier.

To prepare a suitable stable, dry flavored and aromatic product to which a flavored / flavored frozen product has been incorporated (with or without CO 2), such frozen product is first mixed at low temperature with a solution of suitable solids, then frozen and lyophilized. The solids added to the frozen provide a separating and supportive matrix for flavors and aromas in the dry product in much the same way as the CO2 matrix in the frozen product containing CO2.

16 58047

Suitable solids that can be added to the "frozen" in solution form include a wide variety of substances, typically carbohydrates such as saccharides, oligosaccharides, hydrolyzed cellulose, cereal extracts, starches, etc., or proteins. One particularly suitable solid is a conventionally prepared soluble solid from the same or similar type of substrate that was extracted to obtain a flavored / flavored frozen product. Using, for example, solid portions of conventionally prepared instant coffee, decaffeinated instant coffee solids, or a product obtained by subsequent hydrolysis from a substrate from which arcms and flavors have been removed, are particularly suitable. A suitable way to prepare a hydrolysed product for addition to a frozen flavor is to extract the slurry in question. the substrate in the conventional manner after removal of volatile flavors and aromas (recovered as a frozen in the present invention) and the spice concentrate described above (i.e., the liquid removed from the column after bursting). The coffee flavor / flavor frozen can also be added to a solid portion of a cereal product to make a coffee-like product or to a solid portion of milk to make a dry "cream" coffee product. It will be appreciated that a similarly large number of solids may be added to flavored / flavored frozen foods other than substrates.

Sufficient solids must be used to immerse flavors and aromas in the frozen food. Generally, using a CO 2 rinse and one trap of 100 g of finely ground coffee substrate gives about 2 g of a flavored / flavored frozen food, of which about 1800 mg is water and CO2. The remainder is believed to consist of a complex mixture of about 190 mg of highly acidic organic acids (such as fatty acids, citric acid, etc.) and about 10 mg of complex phenols such as chlorogenic acids and their degradation products. It is recommended to add about 2 g of solids to this amount of flavored / flavored frozen; the concentration of such solids should be 10-60% and preferably about Uo% to minimize the amount of water that must be removed in the next freeze-drying. In addition, and as is well known in the art, the use of a high initial concentration of solids in a lyophilized flavored solution results in less loss of spices and flavors.

If desired, lipids (e.g., coffee oil when treating coffee substrates) may also be added in small amounts (e.g., about 0.25% by weight of other solids) as "solids" to stabilize the final product. While not wishing to be bound by any theory, lipids appear to form complexes with flavors and spices and provide more stability therein.

The mixing of the flavored / flavored frozen product and the solids solution should be carried out at the lowest practical temperature, e.g. about 10 ° C in the case of coffee. It is natural for all CO 2 to be removed at the temperatures necessary to dissolve the flavors and flavors in the solid solution.

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It is recommended that the solution of solids be mixed with the "frozen" before the mixture melts, which reduces the mixing that must be done in the liquid phase. The resulting solution should be frozen immediately to preserve taste and aroma.

The result of freezing solids, such as coffee solids, is essentially crystals of pure ice and crystals of solutions of water and solids. As is the case with freeze-drying, "slow freezing" (i.e. relatively high temperatures »about -1 * 0 ° C) can be used to form crystals of water (ice) and solids with a higher density than that achieved by" fast "freezing. A heavier structure is desirable as is known in the art in order to minimize the exposed area and thus evaporation losses, oxidation, etc. Slow freezing is particularly important in the practice of this invention, as the product of the process described above is particularly concentrated for volatile aromatics and therefore particularly sensitive. for all processing conditions.

After freezing, the frozen dry matter / flavor / aroma material is freeze-dried by conventional methods to obtain a stable, solid material containing very large amounts of flavor and aromatic substances. Freeze-drying methods that reduce the exposure time of the product to high temperatures (e.g., vibration-freeze-drying) are particularly recommended.

The following examples illustrate the preparation of the stable, dry, highly aromatic flavored products of this invention.

Example 8

The coffee blend, typically used in the manufacture of vacuum-packed coffee, was ground to a grinding size between about 0.3-0.6 mm under liquid nitrogen (temperature about -60 ° C). 10 kg of this roasted and ground coffee and 100 g of ground solid carbon dioxide were placed in a jacketed extraction column 30.5 cm in diameter and 91 cm long. The column was kept under vacuum in about 1 tower by means of a vacuum pump which drew the vapors down through the column and out through a trap at -195.8 ° C. About 100 ° C of water was fed from the top of the column in bursts (about 333 ml / pulse every two minutes) and turned to a moist steam as soon as it entered the column. The steam condensed on the surface of the lobe particles, wetting them. The vapors removed from the column condensed into a trap, and after about 10 kg of hot water had been fed to the column, an outbreak occurred (i.e., brown liquid began to brick from the column). Prior to onset, approximately 200 g of frozen flavor was collected in a cold trap.

Continuing the hot water supply caused the liquid flavor concentrate of the coffee solids to come from the column. This was collected separately at -76 ° C to give about 12 g of a mild, pleasant instant coffee extract with an apparently pleasant aroma and a concentration of about 17%. When the liquid extract was diluted with about 25 parts per part of the extract, a cup of clear, 18,58047 mild coffee was obtained.

180 g of the above coffee extract (200 g of dry matter) was added to 200 g of Arani / flavored frozen and the mixture was warmed to about 5 ° C to melt to give a solution which was then frozen at -Uo ° C (ambient temperature). ) and lyophilized. 25 mg of the obtained lyophilized product was added to 1 g of a solid obtained by lyophilizing the coffee extract (flavor concentrate) prepared above. When the mixture was added to 150 ml of hot water, a cup of coffee was obtained which was very aromatic in nature and pleasantly tasty, but still not bitter.

Example 9

The procedure of Example 8 was repeated except that the frozen was collected in three fractions of the first, second and third halves before the onset. The drink, made from the first third of the frozen food, had fresh and "high" aromas. The drink made from the last third of the frozen was high and strong but still bitter. The drink, made from the middle third of the frozen, tasted between the other two fractions.

As demonstrated in this example, it is apparent that the process of this invention can be adjusted to produce excellent products suitable for a variety of flavors.

Example 10

Plain Robusta coffee, which typically results in a bitter, coarse rubbery coffee cup in nature, is roasted and ground and processed in the same manner as in Example 8. Surprisingly, a coffee cup made from flavor concentrate extract or flavor concentrate extract and aroma / flavor package which closely resemble those obtained with more expensive mixtures, such as those used in Example 8.

Example 11

The procedure of Example 8 is repeated except that all 12 kg of flavor concentrate (20 x 0 g of dry matter) is added to 50 g (l / l +) of frozen food. This corresponds to the flavor concentrate / frozen ratios in the final product of Example 8. Freeze-drying gives a dry product which, when diluted with 1 g / 150 ml of water, gives a pleasant cup of coffee having the same properties as obtained in Example 8, but slightly milder. It is believed that a higher ratio of water (which is removed in freeze-drying) to flavors and flavors results in an increasing release of most flavors and flavors.

Example 12 50 g of the additional frozen product of Example 11 are mixed with a solution of 50 g of water-soluble soybean protein and 75 g of cold water, and the mixture is frozen and lyophilized. The dry product obtained (about 75 g) is added to 3000 g of water-soluble soybean dry matter. When 1-2 g of the resulting mixture is added to 150 ml of hot water, an excellent, clear coffee-like, nutritious beverage is obtained.

Example 13

The procedure of Example 12 is repeated except that the decaffeinated soluble coffee solids is used instead of the soybean dry matter. Improved decaffeinated coffee is obtained and essentially no caffeine is consumed from the flavored / flavored frozen.

An excellent decaffeinated product is also obtained when a flavored / flavored frozen product is recovered from decaffeinated coffee beans.

Claims (3)

20 58047 A process for preparing a stable, concentrated, strong-tasting, aromatic product from a flavor-containing substrate, wherein said substrate is maintained at a temperature of about 0-60 ° C and extracted by slowly feeding moist steam to a column containing the substrate in a manner that prevents flooding of the column. , while maintaining the column at an absolute pressure of about 0.1-200 mmHg, characterized in that a residue of flavor concentrate is first recovered from the extract by condensing at a temperature of about -80 ° C to -200 ° C before the liquid fraction separates from the column, which is removed and mixed if desired protein and / or carbohydrate solution, and the resulting mixture is frozen and lyophilized, and then a separate flavor and flavor concentrate is collected which concentrates at a temperature in the range of about -80 to -200 ° C, which separate flavor and flavor concentrate is fractionated to a flavor concentrate if desired. who collect by a cold trap having a temperature of about -80 ° C and a second flavor concentrate which is collected by a second cold trap having a temperature of about -200 ° C. Process according to Claim 1, characterized in that the column containing the substrate is purged with an inert gas before and / or during the supply of moist steam. Method according to Claim 1, characterized in that the steam is fed in steps downwards through a column containing the substrate. U. A method according to claim 1, characterized in that the substrate is roasted and ground coffee.