Method for producing a hop extract emulsion, hop extract emulsion produced herewith, food and corresponding uses

Abstract

The invention relates to a method for producing a hop extract emulsion, at least having the following steps: providing a hop extract, mixing the hop extract with water, wherein the mass ratio of water to hop extract is 40:60 to 95:5 (water:hop extract), and homogenising the resulting mixture using ultrasound, which results in the hop extract emulsion. The invention furthermore relates to the hop extract emulsion produced according to the invention, beverages and food produced herewith and corresponding uses.

Description

[0001] Description

[0002] Process for the preparation of a hop extract emulsion, hop extract emulsion prepared thereby, foodstuffs and corresponding uses

[0003] Technical area

[0004] The invention relates to a process for producing a hop extract emulsion according to claim 1, a hop extract emulsion produced therewith according to claim 11, a food product produced therewith or a precursor thereof according to claim 13, and the uses according to claims 14 to 18.

[0005] State of the art

[0006] Hops and hop products made from them have a wide range of applications, the vast majority of which are found in beer production. The bitterness and aroma properties of hops describe the intended use of hops and the hop products made from them. Hop products exist for both of these purposes, used both in the hot section of the brewhouse and in the cold section of the cellar or for filtration. In recent years, hop-aromatic beers have been in increasing demand. This development has given rise to the need to provide brewers with products that are as user-friendly as possible and offer optimal availability of the aromatic compounds.However, with conventional aroma-rich hop extracts or corresponding emulsions, demixing and separation of these products into two or more phases has been repeatedly observed during storage, which is why the storage stability of such products still represents a problem.

[0007] Object of the invention It is therefore an object of the present invention to provide a process which allows the production of a hop extract emulsion which does not visibly demix when stored for several months at 5 to 10°C, i.e. which does not show any phase separation visible to the eye despite storage for several months at 5 to 10°C. It is a further object of the present invention to provide a corresponding hop extract emulsion. Furthermore, it is an object of the present invention to provide a food produced with the hop extract emulsion or a precursor therefor and corresponding uses.

[0008] Definitions

[0009] For the purposes of this invention, the term “α-acids” includes non-isomerized and isomerized α-acids.

[0010] In the context of this invention, “storage-stable” or “long-term storage-stable” is understood to mean the property of an emulsion according to which, when the emulsion is stored at a temperature between 5 and 10 °C for a period of at least 12 months from the time of preparation of the homogeneous emulsion, no demixing of the emulsion occurs to form two phases that would be visible to the eye.

[0011] Summary of the invention

[0012] The above-mentioned object is achieved by the subject matter of the independent claims. Advantageous embodiments of the present invention are the subject matter of the dependent claims.

[0013] From a process engineering point of view, the object is achieved by the process according to claim 1. Thus, a process for producing a hop extract emulsion is claimed, comprising at least the steps: (k) providing a hop extract, preferably a CCh extract or an ethanol extract or a mixture of a COi extract and an ethanol extract;

[0014] (l) mixing the hop extract with water, wherein the mass ratio of water to hop extract is from 40:60 to 95:5 (water:hop extract), preferably 40:60 to 90:10, in particular 50:50 to 70:30; and

[0015] (m) homogenizing or emulsifying the mixture resulting from step (1) using ultrasound, ie introducing ultrasound into the mixture, resulting in the hop extract emulsion.

[0016] In the process according to the invention, it can optionally be provided that any solids present that are not emulsifiable are separated from the hop extract emulsion according to the invention before storage or use. Particularly advantageously, the separation of the non-emulsifiable solids can be carried out after cooling the hop extract emulsion to a temperature between 0 and <5 °C.

[0017] The hop extract emulsion according to the invention resulting from step (m) of the process according to the invention is surprisingly stable over a long period of time, namely at least 12 months, when stored at a temperature between 5 and 10 °C. This property does not separate the homogeneous emulsion to form two phases that would be visible to the eye. This property is also referred to below as "storage-stable" or "long-term storage stability."

[0018] Furthermore, the hop extract emulsion according to the invention obtained by the process according to the invention can be easily dissolved in hot wort or cold beer, water, or other aqueous media with high yield. This allows the hop extract emulsion according to the invention to be used without difficulty in all areas of brewing, beverage production, or in the production of other foodstuffs, particularly as an additive to precursors or to the final product of beverages and foods. This applies particularly when the flavoring properties of hops are the intended use.

[0019] Surprisingly, water, preferably drinking water, process water, or brewing water, especially demineralized brewing water, is sufficient to produce the homogenized hop extract emulsion. No further additives are required to achieve the homogeneity and the long-term storage stability of the hop extract emulsion described above. Therefore, according to the process according to the invention, the hop extract emulsion according to the invention can be limited to the components water and hop extract, and no other ingredients other than hop extract and water are used in the entire process for producing the hop extract emulsion.

[0020] Furthermore, when using the hop extract emulsion according to the invention, due to the fact that the starting material for the process according to the invention is a hop extract, little to no solid ballast, especially hop trub, is introduced into the brewing process, which would then have to be laboriously removed from the wort or beer at another point. This provides a further advantage: the otherwise high loss of wort or beer (up to 30% beer loss in the cold area is possible) during the separation of hop trub can be effectively avoided due to the excellent solubility of the hop extract suspension according to the invention.

[0021] The inventor has further discovered that the mixture of hop extract and water can be easily homogenized or emulsified over the entire mass ratio range from 40:60 to 95:5 (water:hop extract), producing a storage-stable emulsion. If the mixture of hop extract and water contains more than 60% hop extract, spontaneous or temporary demixing was observed; therefore, with more than 60% hop extract in the mixture, long-term storage stability within the meaning of the invention is currently not achievable (see also Fig. 5 and the associated description). With a mass fraction of hop extract of less than 10%, in particular less than 5%, the production of a homogeneous, storage-stable emulsion is technically feasible, but becomes economically unattractive as the water content increases.

[0022] A mass ratio range of 40:60 to 70:30 (water:hop extract) or 50:50 to 70:30 has proven to be particularly advantageous, representing a good compromise between homogenization ability, storage stability and economic efficiency.

[0023] The inventor has further determined that optimal homogenization results of the extract-water emulsion can be achieved if homogenization is carried out solely with ultrasound input into the mixture. However, the process according to the invention does not preclude the ultrasound input being supported by stirring or pumping the emulsion, or by both. Accordingly, the process according to the invention can be limited to using exclusively ultrasound for homogenization according to step (m), or exclusively ultrasound and stirring and / or pumping the mixture. However, further measures to achieve or stabilize the homogeneous emulsion are not required and can be dispensed with.

[0024] As a result, the process according to the invention produces a highly enriched, liquid hop aroma product, the hop extract emulsion according to the invention, which can be used directly and undiluted in all stages of beer or beverage production. The hop extract emulsion can be used without prior treatment such as heating or stirring. Depending on the time of use and the process, the yields of hop aroma compounds are generally at least in the range of hop pellets.

[0025] Advantageous embodiments of the method according to the invention are the subject of the dependent claims.

[0026] Thus, in the process according to the invention, the hop extract of step (k) can be obtained by at least the following steps: (a) providing a hop product in the form of a hop cone or hop pellet, preferably type 90 pellets;

[0027] (b) preparing an extract from the hop product, preferably preparing a CCh extract from the hop product using supercritical CO2 or preparing an ethanol extract from the hop product using ethanol;

[0028] (c) at least partially separating a-acids from the extract; and

[0029] (d) preferably at least partially separating β-acids from the extract; wherein step (d) is carried out before or after step (c), preferably after step (c). The extract remaining after carrying out step (c) or (d) is the hop extract.

[0030] Processes for producing a hop product in the form of a hop cone or hop pellets, which lead to the hop products according to step (a), are the usual processes well known to the person skilled in the art.

[0031] Processes for producing an extract from the hop product which can be used for step (b) or (k) of the process according to the invention are known to the person skilled in the art, for example from the specialist book by Forster, Biendl, Schönberger "Hopfen - Vom Anbau bis zum Bier", Fachverlag Hans Carl GmbH, 1st edition, 2012, ISBN 978-3-418-00808-0, pages 135 to 160.

[0032] The at least partial separation of a-acids from the extract according to step (c) can be carried out by any method known to the person skilled in the art, preferably by the methods described in the document US 2011 / 0 287 152 A1.

[0033] Furthermore, the process according to the invention can provide for partial or complete isomerization of the α-acids present in the extract between steps (b) and (c), although this is not absolutely necessary. The options explained above show that the hop extract to be used for the process according to the invention can be obtained in a variety of ways and is not subject to any particular restrictions. After separation of the majority of the α-acids, the proportion of remaining β-acids can become so high that at least partial separation of the β-acids is necessary to ensure homogenization. The inventor has found that the higher the proportion of remaining β-acids, the more difficult complete homogenization in step (m).Therefore, especially in the case of a high proportion of remaining ß-acids, it can be provided according to the invention to set a mass ratio of water to hop extract of greater than 50:50 and up to 90:10, preferably greater than 50:50 and up to 80:20 (water:hop extract) in step (1).

[0034] The at least partial separation of β-acids from the extract according to step (d) can be carried out by any method known to the person skilled in the art, preferably by the method described in the textbook by Forster, Biendl, and Schönberger "Hopfen - Vom Anbau bis zum Bier" (Hopfen - From Cultivation to Beer), Fachverlag Hans Carl GmbH, 1st edition, 2012, ISBN 978-3-418-00808-0, page 176. The inventor has observed that when the β-acids are separated by this method, a portion of the α-acids still remaining in the extract is also separated.

[0035] According to the invention, it is preferred to separate a total of at least 90 mass%, better at least 99 mass% or even 100 mass%, of the a-acids from the extract in steps (c) and (d).

[0036] Furthermore, the method may comprise the following step:

[0037] (e) separating the extract remaining after step (c) or (d) by distillation, the distillation residue obtained after carrying out step (e) being the hop extract.

[0038] By distilling the hop extract according to optional step (e), it is possible, if desired, to process a hop extract partially depleted in hop oils using the process according to the invention. The hop extract based on the distillation residue, which can be obtained using this embodiment of the process according to the invention, can also be homogenized in water, as provided by the invention. Due to the depletion of hop oils, the resulting emulsion is preferably not used for beer flavoring. Surprisingly, this hop extract emulsion is excellently suited as a natural foam inhibitor. For example, the product can be added to the wort in the brewhouse to prevent excessive foaming of the wort during boiling. Furthermore, this product can also be added to the wort during fermentation to reduce or prevent foam formation in the fermentation tank.

[0039] Furthermore, in the process according to the invention, the α-acids contained in the extract can be at least partially isomerized before step (c). This process step can be carried out by any method known to the person skilled in the art, preferably by the method described in the textbook by Forster, Biendl, and Schönberger "Hopfen - Vom Anbau bis zum Bier" (Hops - From Cultivation to Beer), Fachverlag Hans Carl GmbH, 1st edition, 2012, ISBN 978-3-418-00808-0, page 174.

[0040] Furthermore, the process according to the invention can be limited in such a way that no other substance, preferably no other fluid, in particular no other solvent, other than water is brought into contact with the hop extract when carrying out steps (1) and (m) or during the entire process. Furthermore, according to the invention, it is advantageously not necessary to use steam or other emulsifying aids, with the exception of ultrasound, in the process according to the invention, so that the use of steam, for example, to facilitate emulsification, can be excluded in the process according to the invention. In general, according to the invention, contact of the hop extract or the mixture of hop extract and water with steam can be completely avoided. This reduces the thermal stress and thus the risk of a possible reduction in the quality of the hop extract or the mixture.Furthermore, the inventor has found that the separation of a solid layer or solid particles according to the optional steps (n) to (p) as described below is facilitated if the introduction of water vapor into the mixture in steps (1) and (m) is completely omitted.

[0041] Furthermore, in the process according to the invention, the power introduced into the mixture by means of ultrasound can be from 50 to 100 W / kg of the mixture.

[0042] The ultrasound used in homogenization according to the method according to the invention can have a frequency of 16 to 40 kHz, preferably 18 to 30 kHz.

[0043] In the process according to the invention, the duration of homogenization can be from 0.5 to 20 minutes, preferably from 1 to 10 minutes.

[0044] The inventor of the present invention has discovered that by adhering to one, two, or preferably all of the aforementioned ranges with regard to the power introduced into the mixture via ultrasound, the ultrasound frequency, and the duration of homogenization, optimal homogenization of the hop extract-water mixture and the long-term storage stability described above are achieved. If a power of less than 50 W / kg of the mixture is introduced, sufficient homogenization or long-term stability cannot be ensured. If, on the other hand, the power introduced is greater than 100 W / kg of the mixture, the mixture may heat up excessively, and there is a risk of thermally induced quality losses with regard to the hop components of the mixture.With regard to the ultrasonic frequency, the inventor has discovered that resonances occur within the claimed ranges, in particular around 20 kHz, which facilitate the homogenization of the mixture. With regard to the duration of homogenization, in the inventor's experience, sufficient homogenization cannot be reliably ensured with a duration of less than 1 minute, in particular less than 0.5 minutes. There is no technological upper limit to the duration of homogenization, but a limitation to 20 minutes or even 10 minutes has proven to be an optimal compromise between complete homogenization on the one hand and a short process duration and low energy or heat input on the other. A shorter homogenization duration, i.e. 20 minutes or less, preferably 10 minutes or less, is also preferred with regard to the introduction of oxygen into the mixture.

[0045] Furthermore, the process according to the invention can be limited in such a way that the hop extract and the mixture of the hop extract and water each do not exceed a temperature of 70°C, preferably 60°C, preferably 58°C, in particular 50°C, or even fall below these temperatures. Alternatively or additionally, the process according to the invention can be limited in such a way that heating of the hop extract or the mixture of the hop extract and water to a temperature above 70°C, preferably above 60°C, preferably above 58°C, in particular above 50°C, is avoided.

[0046] Limiting the temperature to which the hop extract and / or the mixture are exposed advantageously serves to avoid quality losses due to negative thermal influences and to maintain the high quality of the hop extract. Thus, the inventor has recognized that, using the process according to the invention, the mixture can be homogenized without problems even at higher temperatures of greater than 50°C, such as 55°C, 58°C, or 60°C. However, at temperatures greater than 50°C or, in particular, greater than 60°C, the homogenization effect no longer improves. However, above these temperatures, increased evaporation of valuable aromatic substances, such as hop oils, from the mixture to be homogenized can be observed. This may be undesirable depending on the objective and should therefore be avoided.In any case, the inventor has observed in experiments that, as long as the temperature of the mixture does not exceed 50 °C during homogenization, there is virtually no influence on the contents of the valuable hop aroma oils, such as myrcene, linalool, caryophyllene, and humulene (measured using the EBC 7.12 method), in the mixture. Thus, yields of aroma substances (hop oils) in the homogenization mixture of > 95% could be achieved. Therefore, in the process according to the invention, it can preferably also be provided that the water has a temperature of 5 to 30 °C, preferably 10 to 20 °C, when mixed with the hop extract in step (1). This measure can advantageously contribute to keeping the temperature of the mixture or the hop extract emulsion in step (m) at a temperature below 60 °C, preferably below 50 °C, i.e. as low as possible, despite the energy input by the ultrasound.

[0047] Finally, the method according to the invention may be limited in that it further comprises the following steps:

[0048] (n) cooling the homogenised mixture obtained from step (m) to a temperature between 0 and < 5 °C;

[0049] (o) maintaining the temperature of the mixture between 0 and < 5 °C for at least 24 hours; and

[0050] (p) skimming off a layer of solids formed on the surface of the mixture or solid particles from the mixture which have formed during step (n) or (o).

[0051] By further developing the process according to process steps (n), (o), and (p), it is possible to completely and easily separate hop waxes and other poorly soluble components that may not be desired in the hop extract emulsion according to the invention and that are initially homogenized together with the other components of the mixture by the process according to the invention from the homogenized mixture as a floating layer of solids. No further demixing of the homogenized hop extract emulsion occurs, i.e., the remaining components of the mixture remain stable as an emulsion.

[0052] The above-mentioned object is further achieved by a hop extract emulsion produced by the process according to the invention as described above. The advantages discussed above in connection with the process according to the invention apply directly or at least analogously to the hop extract emulsion according to the invention.

[0053] The hop extract emulsion according to the invention has a water content of 40 to 95 mass%, preferably 40 to 90 mass%, in particular 50 to 70 mass%.

[0054] Furthermore, the hop extract emulsion according to the invention is characterized by a low viscosity, namely 5 to 150 mPa s, preferably 10 to 100 mPa s, in particular 20 to 50 mPa s, measured at 20 °C, a shear rate of 120 1 / s, and according to DIN 53019, edition 2008-09. Surprisingly, the low viscosity of the hop extract emulsion according to the invention remains essentially stable throughout the entire storage period and changes only insignificantly (maximum increase: 15%, based on the initial viscosity after completion of homogenization, when stored for 12 months at a temperature between 5 and 10 °C).

[0055] In contrast, conventional hop extracts (concentrates) have a significantly higher viscosity of at least 200, in particular at least 300 mPa-s, measured at 50 °C, shear rate of 120 1 / s and according to DIN 53019, edition 2008-09. At temperatures below 50 °C, these are then partially solid, i.e. insoluble. Due to the lower viscosity of the hop extract emulsion according to the invention compared to these conventional hop extracts, a broad range of applications arises for the hop extract emulsion according to the invention in the hot and especially in the cold areas of the brewery or other food manufacturer. Due to the low viscosity of the hop extract emulsion according to the invention, the solubility in wort, beer or other foodstuffs or their precursors is improved, in particular a solution in a cold medium is only possible at a medium temperature between 0 and 25 °C.Based on the inventor's experience, the conventional hop extracts described above pose major problems with dissolving them, especially in cold media such as cold wort or beer. Details on the determination of viscosity as carried out in the context of the present invention: The measurement was carried out using a Rheomat RI 20 (rotational viscometer), manufacturer: proRheo GmbH, Althengstett / Germany, in accordance with DIN 53019, edition 2008-09. The measurement was carried out using a defined measuring body (No. 3 with a diameter of 14 mm) and a measuring tube (No. 3 with a diameter of 18 mm). For the measurement, the measuring body was immersed in a heatable water bath. The water bath and thus the measuring body were heated to a temperature of 20 °C or 50 °C, depending on the hop extract, and the viscosity was measured on the rotational viscometer at a shear rate of 120 1 / s.The result is given in mPa- s (millipascal seconds) and the measurement temperature (here: 20 °C or 50 °C) and the shear rate (here: 120 1 / s).

[0056] In a preferred embodiment of the hop extract emulsion according to the invention, the sum of the mass fractions of hop extract and water is at least 95%, preferably at least 98%, preferably at least 99%, in particular at least 99.5%, based on the total mass of the hop extract emulsion. In an even more preferred embodiment, the hop extract emulsion according to the invention consists of the hop extract and water.

[0057] In a preferred embodiment of the hop extract emulsion according to the invention, the hop extract emulsion does not show any visually detectable separation into two phases within 12 months from production if the hop extract emulsion is stored at a temperature of 5 to 10 °C.

[0058] The object of the invention is further achieved by a food or a precursor thereof, preferably a beverage, in particular a wort or a beer, which contains the hop extract emulsion according to the invention or was produced using the hop extract emulsion according to the invention.

[0059] Here too, the advantages discussed above in connection with the process according to the invention apply directly or at least analogously to the food, preferably beverage, in particular beer, produced with the hop extract emulsion according to the invention.

[0060] The object of the invention is also achieved by the uses according to the invention.

[0061] Thus, the invention claims the use of ultrasound to produce a hop extract emulsion, wherein the hop extract emulsion contains or consists of a hop extract and water. More specifically, this also encompasses the use of ultrasound to emulsify a mixture containing or consisting of hop extract and water.

[0062] All limitations of the inventive method, the hop extract (extraction and / or pretreatment), or the hop extract emulsion, as discussed in this document, may be used individually or in any combination to limit the uses according to the invention. In particular, the inventive use according to any of claims 14 to 18 may be further specified with one or more of the following optional features in any combination:

[0063] • the mass ratio of water to hop extract is 40:60 to 95:5 (water:hop extract), preferably 40:60 to 90:10, in particular 50:50 to 80:20 or 50:50 to 70:30;

[0064] • the water has a temperature of 5 to 30 °C, preferably 10 to 20 °C, when mixed with the hop extract in step (1);

[0065] • when using ultrasound to produce the hop extract emulsion, the mixture forming the hop extract emulsion consists of the hop extract and water, with no other additives or emulsifying aids, including steam, being added to the mixture;

[0066] • the hop extract is prepared from a hop product according to steps (a) to (d) or (a) to (e) described above, wherein the a-acids contained in the extract are not, partially or completely isomerized before step (c);

[0067] • the hop extract emulsion consists of the hop extract and water;

[0068] • the power introduced into the mixture of hop extract and water by means of ultrasound is from 50 to 100 W / kg of the mixture;

[0069] • the ultrasound has a frequency of 16 to 40 kHz, preferably 18 to 30 kHz;

[0070] • the duration of the ultrasound exposure is 0.5 to 20 minutes, preferably 1 to 10 minutes;

[0071] • during the ultrasound exposure, the hop extract and / or the mixture of the hop extract and water does not exceed a temperature of 70 °C, preferably 60 °C, in particular 50 °C;

[0072] • During the ultrasound treatment, the hop extract or the mixture of the hop extract and water is not heated to a temperature above 70 °C, preferably above 60 °C, in particular above 50 °C.

[0073] According to the invention, the use of ultrasound results in the creation of a homogeneous hop extract emulsion that is stable over the long term. Due to the relatively low energy input and the associated low temperature increase during the input, the use of ultrasound is particularly gentle on the product and, in particular, on the aroma, thus resulting in minimal aroma loss due to steaming or thermal degradation. Furthermore, the advantages discussed above for the process according to the invention and the hop extract emulsion according to the invention also apply analogously to the use according to the invention.

[0074] Furthermore, the invention claims the use of the hop extract emulsion according to the invention as an addition to a food or a precursor thereof, preferably to a beverage, in particular to a wort or beer. This includes, in particular, the use of the hop extract emulsion according to the invention, produced from a hop extract at least partially depleted in α-acids, β-acids, and hop oils, as a defoamer for wort, beer, or other liquid foodstuffs or precursors thereof. The inventor has recognized that the addition of the hop extract emulsion according to the invention or produced according to the invention to the wort before, during, or after the treatment of the wort in the whirlpool, preferably between the knocking out of the wort from the brew kettle and the cooling of the wort in the wort cooler, is particularly advantageous.For example, the inventor has found that when using the hop extract emulsion according to the invention, when added to the wort in a whirlpool, the yield of individual hop oil components can be increased to up to 95%. In contrast, the yields of these hop oil components when using Type 90 hop pellets in a whirlpool were only approximately 50%, even though the same overall oil contents were added to the wort in both approaches (see Table 3 below).

[0075] Furthermore, the hop extract emulsion according to the invention or produced according to the invention can be added to the wort or beer at one or more points in the cold section of the brewery, i.e., from the point of pitching with the yeast until the finished beer is bottled in the containers intended for distribution. This allows valuable hop constituents, especially the hop oil components, to be transferred into the beer in a particularly high yield (see Table 4 below).

[0076] The addition of the hop extract emulsion according to the invention to the wort or beer during the primary fermentation has proven particularly advantageous. The hop extract emulsion can preferably be added at the beginning of the primary fermentation, i.e., between the incorporation of the yeast into the wort and the end of the second fermentation day, preferably during the first 24 hours after incorporation.

[0077] Surprisingly, it has also been found that the inventive use of the hop extract emulsion as described in this document can increase the yield of hop oil components, particularly esters, in the finished beer. This allows the fruity character of the resulting beers to be specifically enhanced and emphasized. Thus, the inventive use of the hop extract emulsion can also be provided for increasing the yield of hop oil components and / or esters in the finished beer.

[0078] Finally, the invention claims the use of the hop extract emulsion according to the invention as a defoamer. With the hop extract emulsion according to the invention, an excellent defoamer effect can be achieved in all types of foodstuffs or their precursors that tend to foam, but also in a variety of other substances, such as products or precursors from chemical, pharmaceutical, peri-chemical, and microbiological production. This applies in particular if the hop extract emulsion was produced from a hop extract at least partially depleted in α-acids, β-acids, and hop oils.

[0079] Furthermore, the advantages discussed above for the process according to the invention and the hop extract emulsion according to the invention also apply analogously to the uses according to the invention.

[0080] The inventor has further discovered the following advantages of the invention described herein:

[0081] When using the hop extract emulsion according to the invention, no vegetative material from the hops enters the beverage or other foodstuffs or any precursor thereof. Furthermore, there is virtually no nitrate entry into the beverage or other foodstuffs or any precursor thereof. Furthermore, no particles are introduced into the final product, such as a beer or other beverage, which would then have to be laboriously removed. Furthermore, the conventional beer losses can be avoided by separating particles and hop trub during dry hopping. Finally, when using the hop extract emulsion according to the invention in the brewhouse (adding the hop extract emulsion according to the invention to the wort), a smaller amount of hop trub occurs in the whirlpool, which facilitates separation and minimizes beer losses. Finally, the hop extract emulsion according to the invention can be used in a simple manner, e.g.through automated dosing in a closed system.

[0082] Examples

[0083] In all approaches A to D described below, the following ultrasound device was used:

[0084] Manufacturer: Bandelin, 12207 Berlin

[0085] Type: Sonoplus HD 4400;

[0086] Ultrasonic generator GM4400 - 400 watts;

[0087] Titanium sonotrode TS 425

[0088] Operating frequency: 20 kHz;

[0089] Approach A: Production of homogenized flavor extract

[0090] A hop extract was prepared conventionally by extraction with CO2 or ethanol. After isomerization and separation of the α-acids from the hop extract, a large portion of the β-acids was also separated from the hop extract using a conventional method (variant A1).

[0091] In an alternative variant (variant A2), a hop extract was produced conventionally by extraction with CO2 or ethanol. After separating the non-isomerized α-acids from the hop extract, a large portion of the β-acids was also separated from the hop extract using a conventional method.

[0092] The resulting hop extract of variants A1 and A2, also referred to here as aroma extract, contains only an insignificant proportion of bittering hop acids, in particular only a maximum of 1 / 3 to 1 / 2 of the original ß-acid concentration. Depending on the hop variety used, the hop extract has a high to very high content of hop oils (15 to 45% by mass). In the experimental batch, the viscous hop extract of variant A1 obtained as described above was mixed with water in a mass ratio of 50:50. The resulting mixture was homogenized with the aforementioned ultrasonic device for 5 minutes at an amplitude of 100% and without pulsation at room temperature (400 watts; 20 kHz). The mixture was not cooled during homogenization. Self-heating of the mixture to approximately 50°C was measured during homogenization.

[0093] On the left, Fig. 1 shows the state of the mixture of hop extract and water before homogenization according to the inventive process (batch A, variant A1). The mixture of hop extract (top; dark brown) and water (bottom) is clearly recognizable as a two-phase system. The right half of Fig. 1 shows the state after carrying out the inventive homogenization using ultrasound under the conditions mentioned above. A single, homogeneous phase in a light beige color is visible, which has flow properties similar to water. Precipitated waxes, which are visible floating on the surface, could be removed by simply skimming after cooling to a temperature between 0 and < 5 degrees Celsius. In the hop extract emulsion, the yield of aromatic substances (hop oils) was > 95% (see Table 1 below).

[0094] In the hop extract emulsion according to the invention produced in this way, no separation of the hop extract emulsion into two phases could be observed even after 12 months of storage at a temperature between 5 and 10 °C, for example at 6 °C.

[0095]

[0096] As can be seen from Table 1, the total oil content in the hop extract emulsion according to the invention was reduced compared to the hop extract used in this approach due to the addition of water according to the mixing ratio. Advantageously, homogenization according to the inventive process had virtually no influence on the relative contents of the valuable hop aroma oils myrcene, linalool, caryophyllene, and humulene (based on total oil, measured using the EBC 7.12 method).

[0097] The process according to the invention in the form of approach A described above results in a highly enriched, liquid hop extract emulsion for direct and undiluted addition to, for example, wort or beer during beer production.

[0098] Approach B: Preparation of homogenized beta extract

[0099] A hop extract was prepared conventionally by extraction with CO2 or ethanol. After isomerization, the α-acids were separated from the hop extract using a conventional method. The β-acids were left in the hop extract (variant B1).

[0100] In an alternative variant (variant B2), a hop extract was produced conventionally by extraction with CO2 or ethanol. The α-acids were separated from the hop extract using a conventional method without pre-isomerization. The β-acids were left in the hop extract.

[0101] The resulting hop extract (variants B1 and B2), also called beta extract here, contains only a negligible amount of bittering hop acids, but still maintains approximately the original beta-acid concentration. Depending on the hop variety used, the hop extract has a medium to high hop oil content. Depending on the hop variety used, the hop extract can be hard and solid or highly viscous, depending on the ambient temperature.

[0102] In the experimental batch, the hop extract of variant B1 obtained as described above was mixed with water in a mass ratio of 50:50. The resulting mixture was homogenized with the aforementioned ultrasonic device for 5 minutes at 100% amplitude and without pulsation at room temperature (400 watts; 20 kHz). The mixture was not cooled during homogenization. Self-heating of the mixture to approximately 50 °C was measured during homogenization.

[0103] On the left, Fig. 2 shows the state of the mixture of hop extract and water prior to homogenization according to the inventive process according to approach B, variant B1. The mixture of hop extract (bottom; brown) and water (top) is clearly recognizable as a two-phase system. The right half of Fig. 2 (bottle) shows the state of the mixture after carrying out the inventive homogenization using ultrasound under the conditions mentioned above and after separation of hard, insoluble lumps with a high concentration of ß-acids that precipitated during homogenization. A single homogeneous phase of light beige color is visible, which has flow properties similar to water.

[0104] The precipitated, light-brown lumps are shown in a beaker in the center of Fig. 2. Furthermore, waxes that remained floating on the surface after cooling to a temperature between 0 and <5 degrees Celsius could be removed by simple skimming. The yield of aromatic substances (hop oils) in the hop extract emulsion was <80% (see Table 2 below). In the hop extract emulsion according to the invention produced in this way, no separation of the hop extract emulsion into two phases could be observed even after 12 months of storage at a temperature between 5 and 10 °C, for example, at 6 °C. As can be seen from Table 2, the total oil content in the hop extract emulsion according to the invention was reduced compared to the hop extract used, also in batch B, variant B1, due to the addition of water. Furthermore, it was observed that the content of ß-acids in the homogenized hop extract emulsion was significantly reduced due to the precipitation of solids. The inventor suspects that hop oils, especially the poorly soluble components caryophyllene and humulene, also adhere to a small extent to the precipitated solids. In contrast, the relative contents of the valuable hop aroma oils myrcene, linalool, caryophyllene, and humulene remained roughly unchanged after homogenization. The inventor attributes the slight differences in the relative contents of the hop aroma oils after emulsification compared to the initial state to the reduced hop oil content due to adhesion to the solids.

[0105] The process according to the invention, in the form of the above-described approach B, produces a medium-enriched, liquid hop extract emulsion for direct and undiluted addition to, for example, wort or beer during beer production. Furthermore, a solid hop product rich in beta-acids could be produced as a by-product in the same approach for further processing.

[0106] Approach C: Production of homogenized, deoiled flavor extract

[0107] A hop extract was prepared conventionally by extraction with CO2 or ethanol. After isomerization, the α-acids were separated from the hop extract using a conventional method. The β-acids were largely removed from the hop extract using a conventional method. Furthermore, 50 to 80% of the hop oil content was separated from the hop extract by distillation (variant CI).

[0108] In an alternative variant (variant C2), a hop extract was produced conventionally by extraction with CO2 or ethanol. The α-acids were separated from the hop extract using a conventional method without pre-isomerization. The β-acids were largely removed from the hop extract using a conventional method. Furthermore, 50 to 80% of the hop oil content was separated from the hop extract by distillation.

[0109] The resulting hop extract (variants CI and C2), also called deoiled aroma extract here, contains only a negligible amount of bittering hop acids and a maximum of 1 / 3 to 1 / 2 of the original beta-acid concentration. Depending on the hop variety used, the hop extract has a very low to negligible hop oil content. Depending on the hop variety used and the ambient temperature, the hop extract can be pasty or semi-solid.

[0110] In the experimental batch, the hop extract of variant CI obtained as described above was mixed with water in a mass ratio of 500:30 (water:hop extract). The resulting mixture was homogenized with the aforementioned ultrasonic device for 5 minutes at room temperature at an amplitude of 100% and without pulsation (400 watts; 20 kHz). The mixture was not cooled during homogenization. Self-heating of the mixture to approximately 50 °C was measured during homogenization.

[0111] In Fig. 3 (top left), the state of the mixture of hop extract and water prior to homogenization according to the inventive process according to batch C, variant CI is shown. The mixture of hop extract (bottom; dark brown) and water (top) is clearly recognizable as a two-phase system. In Fig. 3 (top right), the state of the mixture is shown after 2 minutes of homogenization, and in the bottom left after 5 minutes of homogenization (i.e., after completion of the ultrasonic treatment). In this test batch, it is clear that an ultrasonic treatment of 2 minutes is not sufficient to achieve a homogeneous emulsion. After completion of the homogenization step, non-emulsifiable solids and waxes that were present floating on the surface after cooling to a temperature between 0 and < 5 degrees Celsius could be removed by simply skimming.The homogenized hop extract emulsion, freed from residual solids, is shown in the filled state in Fig. 3, bottom right. A single, homogeneous phase of light beige color is visible, which exhibits flow properties similar to water.

[0112] In the hop extract emulsion according to the invention produced in this way, no separation of the hop extract emulsion into two phases could be observed even after 12 months of storage at a temperature between 5 and 10 °C, for example at 6 °C.

[0113] The process according to the invention in the form of approach C described above results in a hop extract emulsion for direct and undiluted addition to, for example, wort or beer during beer production, which is particularly effective for reducing foam formation in boiling or fermenting wort.

[0114] The antifoaming effect is shown in Fig. 4. In Fig. 4, the glass on the left contains a beer without the addition of the hop extract emulsion according to batch C, variant CI (zero sample), the glass in the middle contains the same beer to which 5 g / hl of the hop extract emulsion according to batch C, variant CI, was added, and the glass on the right contains the same beer to which 10 g / hl of the hop extract emulsion according to batch C, variant CI, was added. The picture was taken 25 seconds after the simultaneous addition of the hop extract emulsion. As can be seen from Fig. 4, the amount of foam decreases with increasing addition of the hop extract emulsion, with a significant reduction in the head of the beer already being observed with an addition of 5 g / hl and especially with an addition of 10 g / hl.

[0115] Approach D: Variation of the mixing ratio of the homogenized aroma extract from Approach A

[0116] In another batch, Batch D, the mass-based mixing ratio of water to hop extract was varied: 40:60 and 30:70 (water:extract). All other settings and characteristics are identical to Batch A, Variant A1, described above. Fig. 5 shows the result of the homogenization test after 5 minutes of ultrasonic treatment: the beaker in the right half of the image contains the batch according to the invention with a mixing ratio of 40:60 (water:extract), which resulted in a homogeneous and storage-stable hop extract emulsion (homogeneous phase with a light beige color).

[0117] The beaker in the left half of the image, on the other hand, contains the non-inventive batch with a mixing ratio of 30:70 (water:extract), which was prepared in exactly the same way except for the different mixing ratio. In this batch, spontaneous demixing occurred immediately after the end of the ultrasonic treatment, resulting in the formation of two clearly recognizable phases (top: dark brown extract phase; bottom: light beige liquid phase). Therefore, a homogeneous hop extract emulsion could not be produced with this mixing ratio.

[0118] A further batch, Batch E, was used to test the yields of hop aroma components that could be achieved in a wort when various hop products were added to the wort during its whirlpool treatment. For this purpose, the hop extract emulsion according to the invention was added to the wort in the whirlpool at the beginning of filling the whirlpool. Analogously, hops in the form of Type 90 pellets and in the form of a hop extract, as also provided in step (k) of the inventive process for producing the hop extract emulsion according to the invention, were added to the wort under the same conditions as in the inventive batch. In all three batches, the addition was carried out in such a way that the same total amount of hop oils (g / hl) was added to the wort in each case. All three hop products used for this batch were made from the same hop variety.The concentrations of the aroma components (terpenes, esters, terpene alcohols, and ketones) in the respective coolant wort were determined using GC-MS according to the in-house method of Hallertauer Hopfenveredelungsgesellschaft mbH, method "HHV 46 - Aroma Substances in Beer." The results are summarized in Table 3 below.

[0119] nn = not determinable

[0120] * = Addition of hop products based on the total amount of hop oils, measured according to EBC 7.10: In the product comparisons, the same amounts of hop oil (g / hl) from the same hop variety were always added.

[0121] ** = Determination of the concentration of the components by GC-MS according to the in-house method of Hallertauer Hopfenveredelungsgesellschaft mbH, method “HHV 46 - Aroma substances in beer”.

[0122] As can be seen from Table 3, the concentrations of hop aromatics, i.e., terpenes, esters, terpene alcohols, and ketones, are significantly higher in the batch in which the hop extract emulsion according to the invention was added to the wort, compared to the batches in which either hop pellets or hop extract were added, and are usually several times higher. From this, it can be concluded that the concentration of the investigated hop aromatics in the wort can be significantly increased by adding the hop extract emulsion according to the invention compared to conventional hop products when added to the wort in a whirlpool, under otherwise identical test conditions, and that the hop extract emulsion according to the invention exhibits good and rapid solubility in wort.

[0123] In another approach, Approach F, the yields of hop aroma components that can be achieved in a canned beer were tested when various hop products were added to the fermenting wort. For this purpose, the hop extract emulsion according to the invention was added to the fermenting wort in the fermentation tank 24 hours after the wort had been pitched with yeast. Similarly, hops in the form of Type 90 pellets were added to the fermenting wort under the same conditions as in the inventive approach. In both approaches, the addition was carried out in such a way that the same total amount of hop oils (g / hl) was added to the wort. The control beer used here was beer that was produced in the same way, in particular from the same wort, but to which no hop product was added during fermentation (control). In this approach, too, the two hop products used were made from the same hop variety.The concentrations of aroma components (terpenes, esters, terpene alcohols, and ketones) in the bottled beer were determined using GC-MS according to the in-house method of Hallertauer Hopfenveredelungsgesellschaft mbH, method "HHV 46 - Aroma Substances in Beer." The results are summarized in Table 4 below.

[0124] nn = not determinable

[0125] * = Addition of hop products based on the total amount of hop oils, measured according to EBC 7.10: In the product comparisons, the same amounts of hop oil (g / hl) from the same hop variety were always added.

[0126] ** = Determination of the concentration of the components by GC-MS according to the in-house method of Hallertauer Hopfenveredelungsgesellschaft mbH, method “HHV 46 - Aroma substances in beer”.

[0127] As can be seen from Table 4, the concentrations of hop aroma substances, i.e. terpenes, esters, terpene alcohols and ketones, in the finished beer can be reduced by the described cold hopping with conventional hop products such as

[0128] Pellet Type 90 significantly increased the hop extract emulsion in the cold range compared to the control beer without hopping. In the batch in which the inventive hop extract emulsion was added to the fermenting wort, even higher concentrations were achieved compared to the batch with Pellet Type 90, up to a factor of 3, depending on the parameter, particularly for the esters. In detail, the highly soluble terpene alcohols linalool and geraniol are present in almost identical concentrations in Pellet Type 90 and the hop extract emulsion, as expected. In contrast, other terpene alcohols, such as nerol, citronellol, and terpineol, which contribute floral and citrus notes to the beer aroma, are measured in increased concentrations in the resulting beer when using the inventive hop extract emulsion, despite similarly good solubility.The explanation for this phenomenon can most likely be found in the so-called biotransformation of terpene alcohols and their precursor substances, which is described in this scientific publication: Takoi K, Koie K, Itoga Y, Katayama Y, Shimase M, Nakayama Y, Watari J. Biotransformation of hop-derived monoterpene alcohols by lager yeast and their contribution to the flavor of hopped beer, Journal of agricultural and food chemistry, 2010 Apr 28;58(8):5050-8.

[0129] Similar observations can be made during cold hopping with conventional pellets, but not to such a pronounced extent as when using the hop extract emulsion according to the invention.

[0130] Furthermore, the ester values ​​in the beer produced with the hop extract emulsion according to the invention were significantly higher. This resulted in a more intense fruity note and a clear preference for this beer from a sensory perspective.

[0131] The inventor made these observations independently of the composition of the respective base wort. The test results presented above demonstrate that the hop extract emulsion according to the invention is excellently suited for increasing the yield and / or concentration of hop oil components in wort or beer.

Claims

Claims Process for producing a hop extract emulsion, comprising at least the steps: (k) providing a hop extract, preferably a CCE extract or an ethanol extract or a mixture of a CCE extract and an ethanol extract; (l) mixing the hop extract with water, wherein the mass ratio of water to hop extract is from 40:60 to 95:5 (water hop extract), preferably 40:60 to 90:10, in particular 50:50 to 70:30; and (m) homogenizing the mixture resulting from step (1) using ultrasound. The process according to claim 1, wherein the hop extract of step (k) is obtained by at least the following steps: (a) providing a hop product in the form of a hop cone or hop pellet, preferably type 90 pellets; (b) preparing an extract from the hop product, preferably preparing a CCE extract from the hop product using supercritical CO2 or preparing an ethanol extract from the hop product using ethanol; (c) at least partially separating a-acids from the extract; and (d) preferably at least partially separating β-acids from the extract; wherein step (d) is carried out before or after step (c), preferably after step (c). wherein the extract remaining after carrying out step (c) or (d) is the hop extract. The method of claim 2, wherein the method further comprises the following step: (e) separating the extract remaining after step (c) or (d) by distillation, wherein the distillation residue obtained after carrying out step (e) is the hop extract. The process according to claim 2 or 3, wherein the α-acids contained in the extract are at least partially isomerized prior to step (c). The process according to any one of claims 1 to 4, wherein, during the implementation of step (1), no other substance, preferably no other fluid, in particular no other solvent, other than water, is brought into contact with the hop extract. The process according to any one of claims 1 to 5, wherein the power introduced into the mixture by means of ultrasound is from 50 to 100 W / kg of the mixture; the process according to any one of claims 1 to 6, wherein the ultrasound has a frequency of 16 to 40 kHz, preferably 18 to 30 kHz.The process according to any one of claims 1 to 7, wherein the homogenization duration is from 0.5 to 20 minutes, preferably from 1 to 10 minutes. The process according to any one of claims 1 to 8, wherein, during the process, the hop extract and the mixture of the hop extract and water each do not exceed a temperature of 70°C, preferably 60°C, in particular 50°C; and / or. wherein heating of the hop extract or the mixture of the hop extract and water to a temperature above 70 °C, preferably above 60 °C, in particular above 50 °C, is avoided.

10. The method according to any one of claims 1 to 9, wherein the method further comprises the following steps: (n) cooling the homogenised mixture obtained from step (m) to a temperature between 0 and < 5 °C; (o) maintaining the temperature of the mixture between 0 and < 5 °C for at least 24 hours; and (p) skimming off a layer of solids formed on the surface of the mixture or solid particles from the mixture which have formed during step (n) or (o).

11. Hop extract emulsion prepared by the process according to any one of claims I to 10.

12. Hop extract emulsion according to claim 11, wherein the hop extract emulsion does not show any visually detectable separation into two phases within at least 12 months from manufacture when the hop extract emulsion is stored at a temperature of 5 to 10°C.

13. Food or a precursor thereof, preferably a beverage, in particular wort or beer, containing the hop extract emulsion according to claim 11 or 12, or produced using the hop extract emulsion according to claim II or 12.

14. Use of ultrasound to produce a hop extract emulsion containing or consisting of a hop extract and water.

15. Use of the hop extract emulsion according to claim 11 or 12 as an addition to a food or a precursor thereof, preferably to a beverage, in particular to a wort or beer.

16. Use according to claim 15, wherein the hop extract emulsion is added to the wort before, during, or after treatment of the wort in the whirlpool, preferably between the wort being knocked out of the brew kettle and the wort being cooled in the wort cooler; or wherein the hop extract emulsion is added to the wort or beer in the cold area of ​​the brewery, preferably between pitching the wort and before filtration or bottling of the beer, in particular at the beginning of fermentation.

17. Use according to claim 15 or 16, for increasing the yield and / or concentration of hop oil components in the wort or in the beer.

18. Use of the hop extract emulsion according to claim 11 or 12 as a defoamer.

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