Aroma composition having a grilled-type flavor profile
By heating and atomizing vegetable or animal oils in an anaerobic atmosphere, an aroma composition with unique barbecue-like flavor characteristics is prepared, solving the problems of insufficient aroma characteristics and the formation of undesirable compounds in the prior art, and achieving high-concentration barbecue flavor enhancement and sensory property improvement.
Patent Information
- Application Number
- CN202080105757.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-10-01
- Publication Date
- 2025-11-18
- Estimated Expiration
- 2040-10-01
AI Technical Summary
Existing technologies for preparing barbecue-type aroma compositions suffer from limited aroma characteristics, low flavor concentration, and the formation of undesirable compounds. Furthermore, the preparation process can easily generate harmful substances, requiring additional purification steps.
Vegetable or animal oils are heated to 310°C to 400°C in an anaerobic atmosphere under a pressure of 2 to 5 bar, and then atomized through a nozzle to form an aerosol. The aroma composition is then collected or adsorbed to avoid oxidation and reduce the formation of unwanted compounds.
This resulted in an aroma composition with unique barbecue-like flavor characteristics, enhancing fatty, smoky, roasted, and animalic flavors, reducing waxy flavors, avoiding additional purification steps, and improving aroma concentration and sensory properties.
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Figure CN116323881B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present invention relates to a method of preparing an aroma composition having a grilled-type flavour profile. The present invention also relates to an aroma composition obtainable by the method, and the use of the aroma composition for providing or enhancing a grilled-type flavour and for preparing a food product, a food supplement or an animal feed. The present invention further relates to a food product, a food supplement or an animal feed product itself comprising the aroma composition having a grilled-type flavour profile. Finally, the present invention relates to an apparatus for preparing the aroma composition. BACKGROUND
[0002] In the food industry, various types of flavours are widely used. In savoury foods, aroma compositions having a grilled-type flavour profile are widely used to impart a grilled or charred note to food products for taste purposes.
[0003] The imitation or evocation of the grilled flavour of grilled foods is popular in the food industry and is commonly referred to as "grilled flavour" or "grilled-type flavour". Aroma compositions having a grilled-type flavour profile are suitable to imitate the flavour typically formed by exposing grilled meat products made of meat proteins, meat carbohydrates and animal fat to temperatures, typically by a so-called Maillard reaction. Depending on the chemical composition of the food, the temperature, the cooking time and the presence of air, the Maillard reaction can produce hundreds of different flavour compounds. These compounds often in turn decompose to form even more new flavour compounds.
[0004] Grilled-type flavours are used to impart a highly flavoured grilled note to pre-prepared foods without the need for actual grilling of the food. Grilled flavours also help to incorporate grilled flavour inside many foods that cannot be grilled in other ways, thus serving to enhance grilled flavour without burning or charring.
[0005] Typical grilled flavours include those used to prepare products in which the meat content is reduced or absent, such as sauces, snack foods, meat substitutes, pet foods, etc. Such seasoning compositions can be sprayed onto the food product, or the food can be immersed in a seasoning solution, or the seasoning can be applied in various other ways.
[0006] Grilled-type flavours obtained by pyrolytic reactions and methods for their production are known in the prior art.
[0007] GB 2 363 967 (Colm Declan Menton) describes a method for preparing a grilled flavour comprising the steps of heat treating sunflower oil to prepare a flavour concentrate, and mixing the flavour concentrate with sunflower oil.
[0008] A known barbecue seasoning described in EP 0 867 122 A1 (Ensyn Technologies Inc.) is obtained by heating a spray or atomized droplets of saturated or partially saturated vegetable oil to a temperature of at least 480°C in a fast pyrolysis reactor under an oxygen- depleted atmosphere.
[0009] WO 2019 / 141357 A1 (Symrise AG) discloses a flavoring material substance composition having a grilled aroma profile and a process for its production, the flavoring material substance composition comprising (a) at least five linear or branched saturated aliphatic C5-C16 monocarboxylic acids and (b) at least two a,b-unsaturated C10 aldehydes. In the process for preparing the flavoring material, a plant or animal oil or fat or a mixture thereof is heated to a temperature of 80°C to 300°C at a pressure of 0 to 5 bar for 0.1 seconds to 6 seconds, the resulting product is cooled, and the resulting liquid flavor composition is collected.
[0010] A common typical feature of most of the processes described in the prior art is that the pyrolysis or thermolysis is carried out in an inert atmosphere or in the presence of oxygen or air, for example by purging with air.
[0011] However, the products obtained using such processes generally have a limited aroma profile and a limited level of flavor intensity. In particular, the processes described in the prior art are characterized by the fact that the aroma or flavor composition is prepared at high temperatures, typically at least 350°C, and in the presence of oxygen. Under such drastic conditions, the flavoring oil or fat undergoes very undesirable physicochemical changes, such as oxidation of the double bonds in the fatty acids, or condensation of glycerol with the decomposition fragments of the fatty acids, to name a few. As a result, the resulting oil and fat have a deep yellow-brown to dark brown color and an aroma and taste similar to used frying oil. These aromas and tastes are undesirable because, on the one hand, they impart a gasoline, tar or acid-rancid note to the aroma composition, and on the other hand, they can pose a health hazard. Frying fats have been identified as a source of toxic products such as, for example, polycyclic aromatic hydrocarbons that can form during the pyrolysis or combustion of fats at temperatures above 400°C. For this reason, the processes of the prior art require additional and complex purification steps to isolate or eliminate these undesirable substances.
[0012] Therefore, there is a persistent need for a novel method of producing aroma compositions with barbecue-like aroma characteristics. Another objective of this invention is to provide novel aroma composition products that mimic or evoke a barbecue-like flavor. There is also a strong need to provide a novel aroma composition with improved barbecue-like flavor characteristics. Yet another objective is to improve upon and / or overcome the defects identified in known barbecue seasonings. Finally, yet another objective is to provide products with improved barbecue-like flavor characteristics.
[0013] Therefore, the main objective of this invention is to provide a method for producing an aroma composition that exhibits a novel, enhanced, harmonious and balanced barbecue flavor profile, and prevents or reduces the formation of undesirable flavor compounds such as undecane, heptane, 2E-octene, 1-nonene, cyclooctene and nonadecane.
[0014] Therefore, another object of the present invention is to provide an aroma composition that exhibits novel, intensified, harmonious, and balanced barbecue-like flavor characteristics. In particular, the aroma composition should produce and / or enhance fatty / oily and / or smoky and / or roasted and / or caramelized and / or animalic flavors, while simultaneously suppressing and / or reducing waxy flavors.
[0015] Another object of the present invention is to provide an apparatus for preparing the aroma composition of the present invention having barbecue-like flavor characteristics.
[0016] It has been unexpectedly observed that the following method produces a novel and improved aroma composition with a uniquely distinct barbecue flavor profile: vegetable oil, animal oil, fat, or mixtures thereof are heated to a temperature of 310°C to 400°C at a pressure of 2 bar to 5 bar in the absence of air or oxygen in the reaction zone (i.e., no air or oxygen supply), and subsequently atomized through a nozzle. This barbecue flavor profile is predominantly characterized by an extremely high proportion of fatty / oily and / or smoky and / or roasted and / or caramelized and / or animalic flavor profiles, and a reduced amount of waxy flavor profiles. This barbecue flavor differs from the flavor profiles or characteristics of aroma compositions achieved using methods according to the prior art, even when using the same raw materials.
[0017] According to the present invention, "flavor profile" means one or more compounds that produce the flavor components of the aroma composition according to the present invention.
[0018] The unique flavor profile and enhanced (i.e., higher) concentration of this barbecue-style seasoning indicate that this method produces a distinct new composition. This type of unique barbecue seasoning is highly suitable for the food seasoning industry because the desired flavor can be achieved using reduced amounts of seasoning (additives). Furthermore, a more pronounced flavor can be achieved using the same amount of other barbecue seasonings.
[0019] It has also been surprisingly discovered that the method according to the invention prevents or reduces the formation of undesirable flavor compounds such as undecane, heptane, 2E-octene, 1-nonene, cyclooctene, and nonadecane (which impair the sensory properties of the aroma composition), making the manufactured aroma composition usable directly without additional purification steps. Summary of the Invention
[0020] In a first aspect, the present invention relates to a method for preparing an aroma composition having a barbecue-like flavor profile, the method comprising or consisting of the following steps in sequence:
[0021] (a) Provide vegetable oils or animal oils or fats or mixtures thereof;
[0022] (b) The product from step (a) is transferred to a reactor and heated to a temperature in the range of 310°C to 400°C, particularly 350°C to 380°C, and a pressure in the range of 2 bar to 6 bar to obtain an oil flow.
[0023] (c) The oil flow is atomized by an atomizing device, preferably by a nozzle, thereby breaking the oil flow into a liquid oil phase.
[0024] And aerosols containing aroma compositions with barbecue-like flavor characteristics;
[0025] (d) Transfer the aerosol containing the aroma to the second pipeline and transfer the liquid oil phase to the third pipeline;
[0026] (e) By collecting the aerosol or adsorbing the aerosol onto a solid or liquid carrier, the aroma-containing substance is discharged.
[0027] Aerosols; and
[0028] (f) Optionally, the liquid oil phase from step (d) is returned to the reactor.
[0029] In a second aspect, the present invention relates to an aroma composition having barbecue-like flavor characteristics that can be obtained using the method according to the invention.
[0030] In a third aspect, the present invention relates to the use of the aroma composition having barbecue-like flavor characteristics for providing or enhancing fatty / oily and / or smoked and / or roasted and / or caramelized and / or animal flavors in food, food supplements or animal feed and for simultaneously suppressing and / or reducing waxy flavors and / or for use in the preparation of food, food supplements or animal feed.
[0031] In a fourth aspect, the present invention relates to consumer products, food supplements or animal feeds in which the aroma composition according to the invention has been applied.
[0032] Finally, the present invention relates to an apparatus for producing an aroma composition having a barbecue-like flavor profile, the apparatus having a reactor 1 comprising:
[0033] (i) a reservoir 2 for vegetable oil or animal oil or fat or a mixture thereof, a pump 3, and a heater 4 adapted to heat the vegetable oil or animal oil or fat or a mixture thereof to produce a heated oil flow;
[0034] (ii) an atomizing device, preferably nozzle 6, which is adapted to atomize the heated oil stream in order to break the oil stream into a liquid oil phase and an aerosol containing an aroma composition with barbecue-like flavor characteristics.
[0035] (iii) Optionally, inlet 7 is adapted to inject fluid or gas near the nozzle outlet or to apply a vacuum near the nozzle outlet;
[0036] (iv) Second pipeline 9, which is adapted to discharge the aerosol containing the barbecue flavor;
[0037] (v) Third pipeline 10, which is adapted to return the liquid oil phase to the reactor;
[0038] (vi) Container 11, which is adapted to collect the aerosol; and
[0039] (vii) Collector 12, which is adapted to collect the liquid oil phase. Attached Figure Description
[0040] Figure 1 This is a schematic diagram of the device according to the present invention.
[0041] Figure 2a and Figure 2b Each of the above is a schematic cross-section of a preferred embodiment of the nozzle of the device according to the invention, depicting a single-component nozzle, i.e., a straight-forward orifice, without additive gases or the like.
[0042] Figure 3 is a schematic cross-section of another preferred embodiment of the nozzle of the device according to the invention, using additives, typically inert atomizer gas.
[0043] Figure 4 This is a schematic cross-section of another preferred embodiment of the nozzle of the device according to the invention, which is an internal mixing nozzle in which atomizer gas is supplied inside the nozzle.
[0044] Figure 5 This is a schematic cross-section of another preferred embodiment of the nozzle of the device according to the invention, depicting effervescent atomization, which is a special type of atomization.
[0045] Figure 6 This is a schematic cross-section of a preferred embodiment of the venturi nozzle of the device according to the present invention.
[0046] Figure 7 This is a schematic cross-section of another preferred embodiment of the nozzle of the device according to the invention.
[0047] Figure 8 This is a spider diagram showing the flavor characteristics of a barbecue flavor according to the invention compared to the flavor characteristics of a barbecue flavor according to the prior art. It also shows a comparison of the flavor characteristics of a barbecue flavor obtained according to WO 2019 / 141357 A1 with the flavor characteristics obtained according to the invention after four inhalations.
[0048] The present invention is described in detail in the appended claims. However, the invention itself, its preferred variations, other aspects and advantages will become apparent from the following detailed description in conjunction with the appended embodiments and drawings. Detailed Implementation
[0049] The invention will now be described with reference to the accompanying drawings. In the following description, the same reference numerals are given to corresponding elements shown in each of the figures.
[0050] In a first aspect, the present invention relates to a method for preparing an aroma composition having a barbecue-like flavor profile, the method comprising or consisting of the following steps in sequence:
[0051] (a) Provide vegetable oils or animal oils or fats or mixtures thereof;
[0052] (b) The product from step (a) is transferred to a reactor and heated to a temperature in the range of 310°C to 400°C, particularly 350°C to 380°C, and a pressure in the range of 2 bar to 6 bar to obtain an oil flow.
[0053] (c) The oil stream is atomized by an atomizing device, preferably by a nozzle, thereby breaking the oil stream into liquid oil.
[0054] The phase and contain an aroma composition with barbecue-like flavor characteristics in an aerosol;
[0055] (d) Transfer the aerosol containing the aroma to the second pipeline and transfer the liquid oil phase to the third pipeline;
[0056] (e) By collecting the aerosol or adsorbing the aerosol onto a solid or liquid carrier, the aroma-containing substance is discharged.
[0057] Aerosols; and
[0058] (f) Optionally, the liquid oil phase from step (d) is returned to the reactor.
[0059] Figure 1 A schematic diagram of an apparatus according to the invention is depicted. The apparatus includes a reactor 1 of a type suitable for producing aroma compositions with barbecue-like flavor characteristics. Reactor 1 includes a reservoir 2, a pump 3, and a heater 4, in which vegetable oil, animal oil, fat, or mixtures thereof are provided. Reactor 1 also includes a first pipeline 5, an atomizing device, preferably a nozzle 6, a second pipeline 9, a third pipeline 10, a container 11 for the discharged aroma, and a final collection vessel 12 for the liquid oil phase.
[0060] One characteristic of the process according to the invention is that the aroma composition can be produced in a continuous reactor, which enables the continuous production of the flavor composition. Alternatively, the composition can be produced in batches.
[0061] In the first step (a) of the method according to the invention, vegetable oil or animal oil or vegetable fat or animal fat, or a mixture thereof, is provided as a starting product for producing the aroma composition according to the invention. For the purposes of this application, this means that a single vegetable oil or a single animal oil or a single vegetable fat or a single animal fat, or a mixture of two or more of vegetable oil, animal oil, vegetable fat, or animal fat, may be used.
[0062] Vegetable oils and fats are biological mixtures of plant origin, composed of mixtures of esters derived from glycerol with fatty acid chains. The physical and chemical characteristics of oils and fats are greatly influenced by the types and proportions of fatty acids on triacylglycerols. Fatty acids can be classified into categories such as saturated fatty acids, monounsaturated fatty acids (MUFAs), and polyunsaturated fatty acids (PUFAs). The main fatty acids present in vegetable oils and fats are saturated and unsaturated compounds with straight fatty acid chains. The most common are even-numbered compounds with 16 to 18 carbon atoms and a single carboxyl group. Many minor fatty acids may be present in the same plant source, including small amounts of branched-chain acids, cyclic acids, and odd-numbered straight-chain acids. An important common feature of most plant-derived oils and fats is the high percentage of unsaturated fatty acids in triacylglycerols. Generally, the higher the degree of unsaturation of fatty acids in vegetable oils, the more susceptible they are to oxidative degradation. Therefore, it is necessary to understand the fatty acid composition of oils or fats to determine their characteristics and to understand their physical and chemical properties. Safflower oil and sunflower oil contain a healthy mixture of all types of saturated and unsaturated fatty acids. For safflower oil and sunflower oil, the P / S index values associated with their effects on human health are also high.
[0063] Suitable vegetable oils used in the method according to the invention are those with high stability, i.e., those that are saturated or partially unsaturated.
[0064] Examples of suitable vegetable oils for use in the method according to the invention include: unsaturated, saturated, or partially saturated palm oil, palm kernel oil, soybean oil, sunflower oil, peanut oil, olive oil, rapeseed oil, grapeseed oil, canola oil, corn oil, coconut oil, sesame oil, poppy seed oil, safflower oil, pumpkin seed oil, rice bran oil, almond oil, pecan oil, macadamia nut oil, cottonseed oil, flaxseed oil, or mixtures of two or more of these vegetable oils. Alternative ingredients include animal fats, such as pork fat (lard), beef fat (fat), mutton fat (fat), bacon fat, chicken fat, turkey fat, butter, or mixtures of two or more of these animal fats.
[0065] According to Vesna Kostik et al., Fatty acid composition of edible oils and fats, HEDJ Journal of Hygienic Engineering and Design, original scientific paper, UDC 664.3:577.115.3, the contents of the following saturated and unsaturated fatty acids in the tested oil samples are shown in Tables 1 and 2: hexanoic acid (C6:0), caprylic acid (C8:0), capric acid (C10:0), lauric acid (C12:0), myristic acid (C14:0), palmitic acid (C16:0), stearic acid (C18:0), arachidic acid (C20:0), betaine acid (C22:0), ligninic acid (C24:0), oleic acid (C18:1), linoleic acid (C18:2), and linolenic acid (C18:3).
[0066] Table 1: Saturated fatty acid (SFA) composition of different vegetable oils and fats (% w / w)
[0067]
[0068] Table 2: Unsaturated fatty acid (UFA) composition of different vegetable oils and fats (% w / w)
[0069]
[0070]
[0071] The total content of saturated fatty acids (SFA), monounsaturated fatty acids (MFA), and polyunsaturated fatty acids (PUFA), as well as the relationship between the saturated fatty acid content and the polyunsaturated fatty acid content, is expressed as the P / S index. The P / S index is an important parameter for determining the nutritional value of an oil. Oils and fats with a P / S index value higher than 1 are considered to have nutritional value. Safflower oil has the highest P / S index value.
[0072] Table 3: Content and P / S Index (polyunsaturated / saturated index) of saturated fatty acids (SFA), monounsaturated fatty acids (MUFA), and polyunsaturated fatty acids (PUFA) (% w / w) in different types of vegetable oils
[0073]
[0074] Sunflower seed oil showed a high PUFA content (59.5% ± 7.5%), mainly linoleic acid (C18:2). The highest total unsaturated fatty acid content was found in safflower oil (92.6% ± 1.0%) and sunflower oil (91% ± 2.12%).
[0075] The above fatty acid contents and results are consistent with data obtained in the literature (see Zambiazi RC et al., Fatty acid composition of vegetable oils and fats (2007), B. CEPPA, Curitiba (25(1), pp. 111-120 and Daniewski M. et al., Fatty acids content in selected edible oils (2003), Roczniki-Pastwowego-Zaklad-Higieny 54(3), pp. 263-267). However, the data may vary depending on the plant variety, season, origin, etc.
[0076] It has been found that if the oil or fat starting product provided in step (a) contains the following fatty acid profile, a seasoning composition with particularly advantageous sensory barbecue-like flavor characteristics is produced:
[0077] - 3% to 14.0% by weight of palmitic acid (C16:0);
[0078] - 0.8% to 12.5% by weight of stearic acid (C18:0);
[0079] - 18.0% to 87.0% by weight of oleic acid (C18:1);
[0080] - 2.0% to 30.0% by weight of linoleic acid (C18:2);
[0081] - 0.2% to 2.2% by weight of arachidic acid (C20:0); and
[0082] - 0.6% to 4.0% by weight of behenic acid (C22:0);
[0083] And optionally, one or more fatty acids from the group consisting of:
[0084] - 0% by weight to 6.0% by weight of butyric acid (C4:0);
[0085] - 0% to 2.9% by weight of hexanoic acid (C6:0);
[0086] - 0% by weight to 65.0% by weight of octanoic acid (C8:0);
[0087] - 0% by weight to 45.0% by weight of decanoic acid (C10:0);
[0088] - 0% to 4.5% by weight of lauric acid (C12:0);
[0089] - 0% to 11.5% by weight of myristic acid (C14:0);
[0090] - 0% to 74.0% by weight of linolenic acid (C18:3);
[0091] - 0% to 4.3% by weight of eicosenoic acid (C20:1);
[0092] - 0% to 2.5% by weight of cetylene (C22:1);
[0093] - 0% to 2.9% by weight of myristone acid (C14:1); and
[0094] - 0% to 3.9% by weight of palmitic acid (C16:1);
[0095] The above is based on total fatty acid content, provided that the indicated quantities total 100% by weight.
[0096] In a preferred variation, the oil or fat starting product provided in step (a) comprises the following fatty acid profile:
[0097] - 4.0% to 8.0% by weight of palmitic acid (C16:0);
[0098] - 3.0% to 11.0% by weight of stearic acid (C18:0);
[0099] - 72.0% to 85.0% by weight of oleic acid (C18:1);
[0100] - 4.0% to 17.0% by weight of linoleic acid (C18:2);
[0101] - 1.5% to 2.0% by weight of arachidic acid (C20:0); and
[0102] - 2.5% to 3.5% by weight of behenic acid (C22:0);
[0103] The above is based on the total fatty acid content, provided that the indicated quantities total 100% by weight.
[0104] Of the vegetable oils specified above, those with particularly high oleic acid and / or linoleic acid content are preferred as starting products in the method according to the invention. Among the vegetable oils specified above, sunflower oil, rapeseed oil, corn oil, flaxseed oil, and safflower oil are particularly preferred due to their oleic acid (18:1) and linoleic acid (18:2) content. Sunflower oil with a high oleic acid content is especially preferred as a starting product. A known high-oleic sunflower oil has approximately 82% oleic acid.
[0105] Oil or fat starting material or raw material is provided in reservoir 2.
[0106] In a subsequent step (b) of the method according to the invention, a feed stream of the oil or fat starting product is introduced via pump 3 along the first pipeline 5 toward the heater 4, which is provided as a heating or reaction zone. The oil or fat starting product or raw material can be fed continuously or in batches into the heating or reaction zone.
[0107] In the heating or reaction zone, thorough and rapid mixing takes place, and conductive heat is transferred from the heater to the oil or fat starting product or raw material.
[0108] In a heating or reaction zone, the oil or fat starting product or raw material is heat-treated, wherein it is heated to a temperature in the range of 310°C to 400°C. In a preferred variation of the method according to the invention, the oil or fat starting product is heated to a temperature in the range of 350°C to 380°C, and particularly preferably 360°C to 370°C. Unpleasant flavors are produced at contact temperatures above 400°C, while the desired flavor characteristics and the desired concentration of flavor compounds are not produced at contact temperatures below 310°C. The optimal contact temperature is above 360°C but below 370°C.
[0109] Step (b) of heating the oil or fat starting product is carried out at a pressure of 2 bar to 6 bar, and particularly preferably 3 bar to 4 bar. This improves the flow properties and helps control the aroma.
[0110] The residence time of the oil and fat starting products in the heating zone is 10 to 30 seconds, preferably 12 to 28 seconds, and particularly preferably 15 to 25 seconds. Residence time is defined as the time from the time the raw material comes into contact with the heater to the time the raw material leaves the heating zone.
[0111] When the oil or fat starting product is heated to a temperature in the range of 360°C to 370°C for 10 to 30 seconds at a pressure in the range of 3 bar to 4 bar in step (b), an aroma composition with particularly advantageous sensory properties is obtained.
[0112] It has been found that the temperature in step (b) is crucial for obtaining a harmonious and balanced barbecue-style flavor profile with a high impact, namely flavor intensity, particularly where fatty / oily and / or smoky and / or roasted and / or caramel and / or animal flavor profiles are enhanced while waxy flavor profiles are suppressed or reduced.
[0113] Using the process parameters specified above, during the heating step (b) of the method according to the invention, compounds that contribute to fatty / oily and / or smoky and / or roasted and / or caramel and / or animalic flavor profiles, such as decanoic acid, oleic acid, 2E-decenal, 2E-undecenal, 2E,4E-decadienal, and 1-dodecene, are advantageously generated in the oil or fat starting material, while simultaneously inhibiting or significantly reducing the formation of undecane, heptane, 2E-octene, 1-nonene, cyclooctene, and nonadecane, which are detrimental to sensory properties. These subsequent compounds may form undesirable waxy flavor profiles.
[0114] According to the method of the invention, particularly the heating step (b), it is carried out in a reducing atmosphere, which is either at a reduced oxygen level or substantially free of oxygen or air. No air or oxygen is supplied in the pyrolysis or high-temperature decomposition step (b). The only oxygen present is the oxygen necessary to purge the pressure gauge orifice, any residual oxygen in the feedstock, or oxygen that enters the system due to system limitations or leaks.
[0115] In a preferred variation, the heating step (b), i.e., pyrolysis or high-temperature decomposition, is carried out in the absence of oxygen or air in the reaction zone. Preferably, the process is carried out without purging air.
[0116] Preferably, the oil flow generated in the first pipeline 5, which exits the reservoir 2 and passes through the heating zone 4, is laminar. This avoids turbulence, reduces friction, and provides a continuous source for the atomizing device, thereby providing a predictable aroma concentration.
[0117] Because oxygen is absent or nearly absent in the heating or reaction zone, the process of the present invention is endothermic pyrolysis or high-temperature decomposition and is a non-combustion process. This results in a series of entirely different chemical reactions, producing different aroma compositions than those obtained using methods according to the prior art, as exemplified in Table 4 below.
[0118] In the heating or reaction zone 4 of reactor 1, preferably by means of resistance heating, indirect combustion, direct combustion or a combination thereof, the oil or fat starting product or raw material is raised to the desired near temperature.
[0119] In a preferred variation, the oil or fat starting product or feedstock is subjected to high-temperature treatment in a heated zone in the form of a thin film (i.e., a sheet, flake, or droplet). This maximizes the exposure of the oil or fat starting product to the desired temperature to obtain an aroma composition with the desired barbecue-like flavor characteristics. A preferred method for this high-temperature treatment of the oil or fat starting product is a continuous-feed, thin-film, and / or high-temperature cooking process. Alternatively, rods heated to the desired temperature range can be inserted into the oil or fat bath for high-temperature treatment.
[0120] In a preferred variant of the method according to the invention, the oil or fat starting product or raw material is heated by electromagnetic induction.
[0121] Induction heating processes have been used in industry for a long time and are well known to those skilled in the art. The most common applications are melting, hardening, sintering, and / or heat treating alloys. However, processes such as bonding, shrinking, or joining parts are also well-known applications of this heating technology.
[0122] Technical documents describe the principles of induction heating and the design of induction heating devices, for example: Elektrotechnologie (Electrical Engineering), edited by H Conrad and R Krampitz, VEB Verlag Technik Berlin, 1983, pp. 58-114; (Induction Heating), G. Benkowski, Berlin Verlag Technik, 1990; Practical Induction Heat Treating, R. E. Haimbaugh, ASM International, December 2001; Handbook of Induction Heating, V. Rudnev, D. Loveless, R. Cook, M. Black, Marcel Dekker Inc, New York and Basel, 2003.
[0123] Document DE 10 2005 051 637 describes a reactor system with a microstructured reactor and a method for carrying out chemical reactions in such a reactor. The reactor itself is heated by electromagnetic induction. Heat is transferred to the reaction medium via the heated reactor walls.
[0124] From the journal article “Inductive heating in organic synthesis by using functionalised magnetic nanoparticles in microreactors” by S Ceylan, C Friese, Ch Lammel, K Mazac and A Kirschning (see: Angewandte Chemie 2008(129), pp. 9083-9086, Angewandte Chemie International Edition 2008(47), pp. 8950-8953), it can be seen that chemical reactions can be carried out by means of electromagnetic induction heating media.
[0125] The principles of induction heating and the design of induction heating devices are described, for example, in the aforementioned technical documents, enabling those skilled in the art, who consult available technical documents and apply their common knowledge in the field, to readily install the apparatus for performing the method without excessive effort or inventive steps, and to determine the optimal parameters for induction heating (e.g., the selection of the reactor and inductor frequencies) to perform the process over the entire range under consideration.
[0126] In a preferred embodiment of this application, the reactor wall itself is heated. Therefore, the reactor is composed of a conductive and / or magnetizable material that heats up under the influence of an alternating electromagnetic field. Preferred reactor materials include conductive ceramics, such as SiC (silicon carbide), or preferably refractory metals selected from the group consisting of titanium, tantalum, niobium, molybdenum, tungsten, alloys of these metals, nickel-based, cobalt-based, and chromium-based alloys, and high-temperature resistant steels.
[0127] However, within the scope of this invention, heat transfer elements such as heating coils or heat exchanger tubes or plates may also be incorporated into the reactor.
[0128] Undoubtedly, the properties of the heating medium and the design of the inductor must be compatible to achieve the desired heating of the reaction mixture. For this purpose, key parameters are the inductor's power in watts and the frequency of the alternating field generated by the inductor. In principle, the greater the mass of the heating medium to be inducted, the greater the power required. In practice, the achievable power is particularly limited by the cooling capacity of the generator needed to power the inductor.
[0129] Inductors that generate alternating fields with frequencies ranging from about 1 kHz to about 100 kHz, preferably from about 10 kHz to about 80 kHz, and particularly preferably from about 10 kHz to about 30 kHz are particularly suitable. Such inductors and associated generators are commercially available, for example, from IFF GmbH in Ismaninger, Germany.
[0130] Therefore, induction heating is preferably performed using an alternating field in the mid-frequency range. Compared to higher frequency excitations, such as those in the high-frequency range (above 0.5 MHz and particularly above 1 MHz), this induction heating has the advantage of better control over the energy input to the heating medium. Therefore, in the context of this invention, it is preferable to use an inductor that generates an alternating field in the aforementioned mid-frequency range. This allows for economical and easy control of the reaction.
[0131] To prevent heat loss to the reactor due to convection or conduction through air, the reactor can be housed in a vented enclosure. This applies to all types of reactors that can be used in the process of this invention. The vented enclosure provides the additional advantages that any leaks in the reactor can be easily detected analytically or rapidly due to pressure build-up within the enclosure. It also prevents toxic compounds escaping through leaks from directly entering the atmosphere.
[0132] The reactor shell can be, for example, an elongated glass, quartz glass, or ceramic shell. This shell may have an internal heat-reflective cover to minimize losses due to heat radiation. The coating is preferably not composed of conductive materials to prevent temperature rise during induction heating using an energy field. Additionally or alternatively, a heat-reflective inner coating may also be disposed in the venting area and may be made of the same material as the heat-reflective coating on the reactor shell. The shell may also be self-cooled, for example, using water or air.
[0133] Once the oil or fat starting material is heated under the above conditions, a heated and pressurized oil stream containing pyrolysis products is obtained, and the oil stream leaves the heating or reaction zone.
[0134] In process step (c), the heated and pressurized oil stream containing pyrolysis or high-temperature decomposition products is then piped through the first line 5 to an atomizing device, which may be a nozzle 6, for atomizing or vaporizing the heated oil stream and breaking it into a liquid oil phase and an aerosol containing an aroma composition with barbecue-like flavor characteristics.
[0135] Preferably, the oil flow produced by being piped through the first pipeline 5 and leaving the heating zone 4 is laminar. This avoids turbulence, reduces friction, and provides a continuous source for the atomizing device, thereby providing a predictable aroma concentration.
[0136] The term "atomization" refers to the separation of matter into fine particles; it is the process of breaking down a large amount of liquid into small droplets, thereby creating an aerosol. An aerosol is defined as a suspension of solid or liquid particles in a gas. Aerosols consist of particles and a suspended gas, typically air. The atomizing device is preferably a nozzle.
[0137] A nozzle is a mechanical device, such as a pipe or tube exhibiting a variable cross-sectional area, where changes in the cross-sectional area affect the interchange of pressure and jet velocity.
[0138] Therefore, in a nozzle, the fluid velocity increases rapidly at the expense of its pressure energy. When a nozzle is placed on a pipe, the flow rate of the nozzle causes a pressure drop, which varies with the flow rate. This can be used for applications such as using nozzles to atomize fluids.
[0139] Typically, the diameter of the nozzle tube gradually decreases from the nozzle's inlet to its outlet. Other designs are possible, but traditionally, fluid or gas is released from a confined tube into free space. At the inlet, the cross-sectional area is large, the pressure is high, and the velocity is low, but towards the nozzle outlet, as the cross-sectional area decreases, the pressure drops and the velocity increases. The ejected driving fluid or power (steam, pressurized liquid, or air) has a fairly high velocity after leaving the nozzle. As the heated and pressurized fluid passes through the nozzle body into free space, a partial pressure drop occurs. Once vapor pressure is reached, evaporation occurs. Due to the pressure difference present, bubbles burst outside the nozzle, exacerbating the disintegration of the heated and pressurized oil flow. This forms two phases: a vapor phase (aerosol) rich in more volatile components and a liquid oil phase rich in less volatile components. The vapor (aerosol) and liquid oil phases are separated by gravimetric analysis. The vapor is carried away in the headspace, while the liquid is discharged to the bottom and exits there.
[0140] Spray nozzles can be classified based on the energy input used to cause atomization, breaking down a fluid into droplets. Spray nozzles may have one or more outlets; multi-outlet nozzles are called compound nozzles. Single-fluid or hydraulic spray nozzles utilize the kinetic energy of the liquid to break it down into droplets.
[0141] According to Bernoulli's principle, when a rapid flow of liquid is injected into the atmosphere through a nozzle, a pressure difference is created between the liquid in the pipe and the lower pressure in the gas flow. The pressure difference between the reduced pressure outside the nozzle and the high pressure inside the nozzle propels the liquid from the first line 5 through the nozzle 6 and into the moving airflow, where the liquid is broken down into small droplets (though not individual atoms, as the term suggests) or atomized. Currently, the atomizer used can be a simple, ordinary orifice nozzle. Such ordinary orifice nozzles include... Figure 2a and Figure 2b As shown.
[0142] Different types of atomizers or nozzles can be used to generate aerosols. Atomizers or nozzles are classified into mechanical atomizers or nozzles or pneumatic atomizers or nozzles based on their energy supply. Rotary or ultrasonic atomizers are classified into the first group. The disintegration of liquids by pneumatic atomizers or nozzles is caused by the aerodynamic interaction between the gas and liquid phases. Jet nozzles, turbulent nozzles, and laminar nozzles are distinguished based on the primary liquid structure on the back of the atomizer or nozzle. The aerodynamic interaction characteristics of two-component nozzles are enhanced by the use of an additional gas.
[0143] Nozzles that rely on atomized fluid without additives are called single-component nozzles. They are characterized by their simple construction. They convert pressure energy into kinetic energy. Turbulent nozzles are also the simplest geometrically formed atomizers. The formation of turbulence in the nozzle is specifically stimulated by guiding the liquid flow within the nozzle. The velocity difference between the surrounding environment and the liquid jet exiting the nozzle causes interactions between the phases. The jet inhomogeneity caused by the turbulence generated in the nozzle is amplified and leads to liquid disintegration. Orifice nozzles or elbow nozzles are examples of the above-mentioned nozzles (see...). Figure 2a and Figure 2b Due to the high mixing rate in the flow, single-component nozzles and turbulent nozzles can provide different aroma characteristics.
[0144] Laminar flow nozzles are used to produce a finer spray at moderate pressures. Unlike turbulent flow nozzles, which form a jet of liquid, laminar flow nozzles are distinguished by the fact that the nozzle shape used shapes the liquid into a laminar flow, which eventually breaks down into droplets. Examples include flat jet nozzles and hollow cone nozzles. These are also currently preferred for providing a larger aerosol distribution compared to the recirculated liquid oil phase.
[0145] In airless atomization, high pressure forces fluid through a small nozzle. The fluid appears as a high-speed solid stream or flake. Friction between the fluid and air disrupts the flow, initially breaking it down into fragments and eventually into droplets. The energy source for this form of atomization is fluid pressure, which is converted into momentum as the fluid leaves the nozzle. Three factors affecting airless spraying include the diameter of the atomizer orifice, the atmosphere, and the relative velocity between the fluid and air. Regarding the orifice diameter, a general rule is that the larger the diameter or size of the atomizer orifice, the larger the average droplet size in the spray. The atmosphere provides resistance and tends to break up the fluid flow. This resistance tends to partially overcome properties such as the fluid's surface tension, viscosity, and density. Air temperature also affects atomization. The relative velocity between the fluid and air also affects droplet size. The fluid velocity is determined by the pressure in the nozzle. As fluid pressure increases, velocity increases and the average droplet size decreases; conversely, as fluid pressure decreases, velocity decreases and the average droplet size increases. In this invention, an airless nozzle can be used.
[0146] Another preferred method to influence droplet size distribution is the use of additives, typically inert atomizer gases. The increased relative velocity between the liquid and gas phases due to the additive gas component increases momentum exchange and creates more intense turbulence in the liquid jet to be atomized. The nozzle geometry depends on the gas supply type. If the gas contacts the liquid to be atomized outside the nozzle, this is called external mixing atomization (see [link to documentation]). Figure 3a and Figure 3b In its simplest case, the liquid is concentrated into a gas jet. The liquid and gas exit the nozzle at different velocities. The momentum exchange between the slower-flowing liquid and the faster-flowing gas accelerates the liquid. These nozzle types with additive gases can be used to atomize oil streams.
[0147] In the case of an internal mixing nozzle, atomizer gas is supplied inside the nozzle (see...). Figure 4 The introduced gaseous components generate turbulence in the multiphase flow, which promotes instability and thus facilitates liquid disintegration. These types are preferred to produce fine aerosol distribution and greater reactor output.
[0148] In air spray atomization, fluid exiting the nozzle at a low speed is surrounded by a high-speed airflow. Friction between the liquid and air accelerates and turbulents the fluid flow, thus causing atomization. The energy source for air atomization is air pressure. The operator can adjust the fluid flow rate independently of the energy source. Figure 4 The fluid flow through the orifice is shown; as the fluid flow occurs, a high-speed airflow surrounds it.
[0149] Effervescent atomization is a special type of atomization in which gas is guided inside. Figure 5 The basic structure of the nozzle is shown. A gas phase is introduced into the mixing chamber. The resulting two-phase flow exists in the mixing chamber as a bubbly flow. A slug flow or annular flow is generated at the nozzle outlet. Outside the nozzle, a thin annular liquid laminar flow is disintegrated into droplets by the high-speed flowing gas phase at the nozzle center. Therefore, this nozzle arrangement is also preferred for achieving better mixing.
[0150] Superheated atomization, or flash atomization, is a special method of generating aerosols. It utilizes a simple pressure nozzle geometry. A liquid stream containing several components partially evaporates in a flash tank under specific pressure and temperature. This forms two phases: a vapor phase (aerosol) rich in more volatile components and a liquid phase rich in less volatile components. The fluid is heated and pressurized before entering the flash tank through a nozzle. As the fluid flows through the nozzle body, a partial pressure drop occurs. Once the vapor pressure is reached, evaporation occurs. Due to the pressure difference, bubbles burst outside the nozzle, further amplifying the disintegration of the liquid stream. Vapor is carried away in the headspace, while the liquid is discharged to the bottom of the tank, exiting from there. Because the vapor and / or superheat phases originate directly from the atomizer liquid, no additional gas additives are needed to disintegrate the liquid. The high temperature of the atomizer liquid reduces its viscosity and surface tension. This promotes the formation of small droplets. As superheat increases, a finer spray is produced. Furthermore, this is a preferred method because it produces finer droplets.
[0151] In a more preferred variation of the method according to the invention, the heated oil stream is atomized or vaporized, and thus broken down into a liquid oil phase and an aerosol containing an aroma composition having barbecue-like flavor characteristics using a venturi nozzle (see [link to venturi method]). Figure 6 ).
[0152] A Venturi nozzle consists of three parts: the nozzle itself, the body, and the diffuser or constriction point. A Venturi nozzle is a mechanical device, such as a pipe or tube exhibiting a variable cross-sectional area, where the change in cross-sectional area affects the exchange of pressure and temperature used for injection velocity. Typically, the diameter of the nozzle tube gradually decreases from the nozzle's initiation point to the constriction point, and then rapidly increases again towards the nozzle's tip (see...). Figure 6 This structure creates back pressure upstream and negative pressure downstream during contraction. As the fluid volume is forced through the narrowing diameter, the laws of fluid dynamics dictate that an increase in velocity is accompanied by a decrease in pressure. Consequently, the jet velocity is very high, coinciding with a rapid drop in pressure and temperature. This process leads to the atomization of the jet fluid.
[0153] Of the above types of nozzles, flash atomization or Venturi nozzles are particularly preferred for use in the method according to the invention.
[0154] The characteristics of the generated aerosol depend to a large extent on the nozzle geometry and the fluid properties of the atomizer liquid. These factors affect the flow rate through the nozzle and the behavior of the droplet clusters after the droplets leave the nozzle. In a capillary, fluid dynamics are determined by changes in cross-section (flow contraction, pressure loss), inhomogeneities (friction), and the properties of the atomizer liquid. Furthermore, several factors influence droplet size and the ease with which the liquid flow atomizes after exiting the orifice. These factors include fluid properties such as surface tension, viscosity, and density.
[0155] The diameter of the nozzle tube in the method according to the invention is preferably 1.2 mm to 3.0 mm, more preferably 1.5 mm to 2.8 mm, and most preferably 2.0 mm to 2.3 mm.
[0156] By atomizing or vaporizing through a nozzle, the heated and pressurized oil stream is broken into two heterogeneous phases: a vapor phase with finer droplets (aerosols) rich in more volatile components that constitute the aroma composition with a barbecue-like aroma profile, and a liquid phase rich in less volatile components. However, the larger droplets in the broken liquid oil phase contain less volatile compounds. The aerosol with finer droplets and the phase with larger oil droplets are separated by gravimetric analysis. The vapor is carried away in the headspace, while the liquid is discharged to the bottom of the tank and exits from there.
[0157] To improve the atomization of the oil flow and thus improve the breaking down of the oil flow into a liquid oil phase and an aerosol containing an aroma composition with barbecue-like flavor characteristics, and / or to increase the velocity of the aerosol flow and thereby accelerate the delivery of the aerosol flow to container 11, the body of the nozzle, preferably a Venturi nozzle, is preferably provided with an inlet 7, such as Figure 7 The illustration is shown in the middle.
[0158] Through this inlet, gas or fluid is injected or drawn into the suction chamber adjacent to the nozzle outlet, thus forming a suction flow. A driving fluid or power source (steam, pressurized liquid, or air) passes through the nozzle of the ejector. By increasing the fluid velocity as it passes through the nozzle, a low-pressure zone, or suction flow, is formed within the ejector at the nozzle outlet. This low-pressure zone entrains and compresses a secondary gas or fluid, i.e., the suction gas or fluid flow. The power flow (steam, pressurized liquid, or air) mixes with the suction gas or fluid flow. As the combined driving fluid and secondary gas or fluid flow pass through the diffuser section of the ejector, the velocity decreases and pressure is regained, causing the fluid to be discharged from the ejector under back pressure.
[0159] In a preferred variation of this method, an inert gas such as nitrogen or air is used as the injection gas for atomization.
[0160] Alternatively, a vacuum is applied to the nozzle or near the nozzle outlet via the inlet 7 to form a suction flow, and this vacuum is controlled by a vacuum control unit 8. The vacuum applied preferably at a pressure of 200 mbar to 800 mbar, more preferably at a pressure of 300 mbar to 600 mbar, and most preferably at a pressure of 450 mbar to 500 mbar, increases the velocity of the motive flow (steam, pressurized liquid, or air) by reducing the pressure.
[0161] The two nozzle configurations described above promote (preferably laminar) atomization of the oil flow and improve the delivery or evacuation of aerosols filled with aroma compositions.
[0162] Therefore, in a preferred variant of the method according to the invention, the atomizing device is characterized by injecting fluid or gas near the nozzle outlet, or applying a vacuum of 200 mbar to 800 mbar pressure near the nozzle outlet.
[0163] The heated and pressurized (preferably laminar) oil stream containing pyrolysis products generated in step (b) of the driving method is passed through any of the nozzles mentioned above, and the oil stream is atomized or vaporized by means of the nozzles, thereby breaking the oil stream into a liquid oil phase and an aerosol containing an aroma composition with barbecue-type flavor characteristics.
[0164] Due to the injection of heated and pressurized fluid into free space, and the resulting partial pressure drop, the aerosol temperature decreases compared to the contact temperature of the oil flow in the heated zone of the reactor. The aerosol temperature near the nozzle outlet is in the range of 180°C to 230°C, preferably in the range of 200°C to 210°C.
[0165] In the subsequent step (d), the resulting aerosol containing an aroma composition with barbecue-like flavor characteristics is discharged along with the stream and transferred to the second line 9. The liquid oil phase separated from the aerosol is transferred to the third line 10.
[0166] In a further preferred variation of the method according to the invention, a vacuum can be applied to the discharge line 9 to create an intake flow or low pressure, thereby accelerating the delivery of the aerosol containing an aroma composition with barbecue-like flavor characteristics to the container 11, and the vacuum is controlled by a vacuum control unit. Preferably, a vacuum is applied at a pressure of 200 mbar to 800 mbar, more preferably at a pressure of 300 mbar to 600 mbar, and most preferably at a pressure of 450 mbar to 500 mbar, which increases the aerosol velocity.
[0167] In the subsequent method step (e), the aerosol containing the aroma composition having barbecue-like flavor characteristics is discharged from the reactor and either collected in a collection vessel or adsorbed onto a solid or liquid carrier.
[0168] Solid carriers are preferably used in the form of finely dried granules or powders. Examples of materials suitable for the food industry include sugars, polysaccharides, and starches (such as potato starch, rice starch, corn starch, etc.), for example, maltodextrin. Other powdered, finely separated food additives / ingredients, such as, for example, silica, can be used. Salts, sugars, and / or flavorings or flavoring extracts are also particularly suitable. The carrier is suitably a liquid carrier. Depending on the end use of the food ingredient, oil-based or water-based carriers are preferred. Water is a preferred carrier. Particularly preferred are oils and mixtures of oils.
[0169] Long shelf life is desirable in food products; therefore, a dry solid carrier in powder form is preferred, and a stable oil is also preferred. Typically, the latter has a relatively low content of polyunsaturated and monounsaturated fats / fatty acids and a high content of saturated fats / fatty acids. The oil preferably has a low level of oxidation.
[0170] The carrier oils suitable for use in this invention include highly stable vegetable oils, i.e., saturated or partially saturated vegetable oils. Preferred oils include: palm oil, soybean oil, peanut oil, olive oil, rapeseed oil, grapeseed oil, canola oil, corn oil, coconut oil, sesame oil, poppy seed oil, safflower oil, pumpkin seed oil, rice bran oil, almond oil, pecan oil, macadamia nut oil, pork fat, beef fat, mutton fat, bacon fat, chicken fat, turkey fat, butter, or mixtures of two or more of these oils and / or fats.
[0171] More specifically, the carrier is preferably an oil with a high saturated fat content: a high level of saturated fatty acids improves stability. Known saturated fat levels are: coconut (approximately 86% to 92%); butter (approximately 50% to 68%); lard (approximately 39%); olive oil (approximately 14%); and sesame (approximately 14%). High levels are those of 10% and above, preferably 30% and above. All these oils can also be used as an oil or fat starting product or as part of an oil or fat starting product. The quality of sunflower oil can also be specifically evaluated based on its oleic acid to linoleic acid ratio. The fatty acid composition of sunflower oil is typically 55% to 65% linoleic acid and 20% to 30% oleic acid, with the remainder comprising other fatty acids, primarily palmitic acid and stearic acid. Sunflower oil is considered a stable oil, and most versions thereof are usable in this invention. Specific versions used in this invention preferably contain even higher levels, particularly at least 50% oleic acid, more preferably at least 60%, and even more preferably at least 70% oleic acid. One known high-oleic sunflower oil contains approximately 82% oleic acid.
[0172] Oils with low saturation levels are generally not well-suited for use as stable carrier oils, but can be acceptable if stability is not a necessary property. These oils include avocado oil, fish oil, flaxseed oil, and some nut oils (including peanut oil).
[0173] Examples of preferred stabilizer carrier oils include oils with high oleic acid content (such as sunflower oil, lard, fat and olive oil), and oils with a saturated fatty acid content of 20% or more, preferably 35% or more.
[0174] In a collecting vessel or by adsorbing the aerosol onto a solid or liquid carrier, the temperature of the aerosol is further reduced, causing it to condense and thereby liquefy. Thus, active cooling of the aerosol is not required in the method according to the invention.
[0175] The concentration of the aerosol in the solid or liquid carrier is at least 0.5% by weight, based on the total weight of the aerosol / carrier composition. Preferably, the aerosol content in the solid or liquid carrier is from 1.0% by weight to 10% by weight or more, based on the total weight of the aerosol / carrier composition. The above range refers to the aerosol content preferably after four cycles.
[0176] Excess reflux liquid oil phase obtained by atomizing and breaking (preferably laminar) the oil flow flows along the third line 10 and is collected in the process oil collector 12. The excess reflux liquid oil phase can be repeatedly recycled to the process oil reservoir 2 by means of a pump.
[0177] The reactor can also operate continuously, which is more efficient.
[0178] Surprisingly, it was found that by repeatedly refluxing the liquid oil phase using the method according to the invention, an aroma composition with barbecue-like flavor characteristics can be achieved, which has a significant influence and enhancement on fatty / oily and / or smoky and / or roasted and / or caramel and / or animalic flavor profiles, but weakens waxy flavor profiles. Two to 25 cycles are possible, with two to six cycles being preferred.
[0179] In a more preferred variation of the method according to the invention, the excess reflux liquid oil phase is recycled 2 to 5 times in undiluted form. In a particularly preferred variation, the reflux liquid oil phase is subjected to the method according to the invention 2 to 4 times. In a most preferred variation, the reflux liquid oil phase is subjected to the method according to the invention 3 or 4 times.
[0180] In continuous operation of the method according to the invention, the cycle time is calculated based on the pumping speed and the time period required for one pass.
[0181] Surprisingly, it was found that if the liquid oil phase was cycled 2 to 4 times in the method according to the invention, compounds contributing to barbecue-like flavor characteristics with fatty / oily and / or smoky and / or roasted and / or caramelized and / or animalic flavor profiles were advantageously obtained, such as decanoic acid, oleic acid, 2E-decenal, 2E-undecenal, 2E,4E-decadienal, and 1-dodecene, as described in Table 4. However, if the liquid phase was cycled 4 to 6 times in the method according to the invention, only a negligible increase in the compounds contributing to barbecue-like flavor characteristics was obtained.
[0182] This has also been confirmed in comparative taste testing, where it was noted that the flavor characteristics of the aroma compositions of the present invention are enhanced, richer, and more concentrated to a greater extent. Figure 7 As shown, the influence of fatty / oily and / or smoked and / or roasted and / or caramel and / or animalic flavor profiles is enhanced, while the waxy flavor profile is significantly weakened compared to the aroma composition of WO2019 / 141357.
[0183] In contrast, in the method according to WO 2019 / 141357, the pyrolytic or high-temperature decomposed oil feedstock is not separated by atomization and thus broken down, but is used as is. However, by the method according to the invention, the pyrolytic or high-temperature decomposed oil feedstock is atomized and thus broken down into two phases. This produces aerosols that are more enhanced and richer in volatile compounds, and advantageously, the aerosols are not diluted with an oil phase, resulting in higher flavor concentrations and thus higher intensity.
[0184] The ratio of the amount of the segregated material (aerosol) rich in the more volatile components that constitute the aroma composition with barbecue-like flavor characteristics to the (recycled) liquid oil phase reaches 1:99, preferably 1:95.
[0185] In a second aspect, the present invention relates to an aroma composition having barbecue-like flavor characteristics that can be obtained using the method according to the invention, as described above.
[0186] Therefore, the present invention relates to an aroma composition having barbecue-like flavor characteristics that can be obtained by a method comprising steps in the following order or steps in the following order:
[0187] (a) Provide vegetable oils or animal oils or fats or mixtures thereof;
[0188] (b) The product from step (a) is transferred to a reactor and heated to a temperature in the range of 310°C to 400°C, particularly in the range of 350°C to 380°C, and a pressure in the range of 2 bar to 6 bar, in order to obtain an oil flow.
[0189] (c) The oil stream is atomized by an atomizing device, preferably by a nozzle, thereby breaking the oil stream into a liquid oil phase and an aerosol containing an aroma composition with barbecue-like flavor characteristics;
[0190] (d) Transfer the aerosol containing the aroma to the second pipeline and transfer the liquid oil phase to the third pipeline;
[0191] (e) Discharging the aerosol containing the aroma by collecting the aerosol or adsorbing the aerosol onto a solid or liquid carrier; and
[0192] (f) Optionally, the liquid oil phase from step (d) is returned to the reactor.
[0193] Preferably, the obtained aroma composition can be combined with a solid or liquid carrier and / or other suitable food additives.
[0194] The aroma compositions with barbecue-like flavor characteristics produced using this invention have a high impact and distinct features. Surprisingly, the aroma compositions according to the invention have a harmonious and balanced barbecue-like aroma characteristic. The aroma compositions according to the invention have improved sensory properties and are characterized by the fact that they provide and / or enhance fatty / oily and / or smoky and / or roasted and / or caramelized and / or animalic flavor profiles, while suppressing or reducing waxy flavor profiles.
[0195] It was also surprisingly found that the manufacturing method according to the invention prevents, inhibits, or greatly reduces the formation of undecane, heptane, 2E-octene, 1-nonene, cyclooctene, and nonadecane, which are harmful to sensory properties.
[0196] As can be seen from Table 4, even using the same raw materials, the aroma compositions described in this application exhibit significantly different flavor profiles from those obtained using the process described in WO2019 / 141357. In particular, in comparative tests, compounds contributing to the formation of barbecue-like flavor characteristics (i.e., fatty / oily and / or smoky and / or roasted and / or caramelized and / or animalic flavor profiles) were enhanced; such compounds include decanoic acid, oleic acid, 2E-decenal, 2E-undecenal, 2E,4E-decadienal, and 1-dodecene, as also seen in Table 4. However, in comparison, the aroma compositions obtained using the process described in WO 2017 / 141357 contain fewer barbecue-like flavors (such as fatty / oily, smoky, roasted, and caramelized flavors), while waxy and soapy aroma components are enhanced.
[0197] The aroma composition produced by the above method can be determined using standard analytical methods such as gas chromatography.
[0198] In particular, the comparative taste test panel noted that the flavor characteristics of the aroma composition of the present invention were further enhanced, richer, and more concentrated. For example... Figure 8 As shown in the spider diagram, compared with the aroma composition of WO 2019 / 141357, the influence of fatty / oily and / or smoky and / or roasted and / or caramel and / or animalic flavor profiles is particularly enhanced, while the waxy flavor profile is significantly weakened.
[0199] The aroma composition with an improved barbecue flavor according to the present invention preferably comprises:
[0200] (a) at least one, preferably two, types of straight-chain or branched, saturated or unsaturated aliphatic C8-C20 monocarboxylic acid;
[0201] (b) at least one, preferably two, types of α,β-unsaturated C6-C14 aldehydes; and
[0202] (c) At least one, preferably two, types of α,β-unsaturated C6-C14 olefins.
[0203] The at least one type of straight-chain or branched, saturated or unsaturated aliphatic C8-C20 monocarboxylic acid is preferably selected from the group consisting of: octanoic acid, nonanoic acid, decanoic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, nonadecanoic acid and eicosanoic acid.
[0204] The at least one type of α,β-unsaturated C6-C14 aldehyde is preferably selected from the following compositions: C6-aldehyde, C7-aldehyde, C8-aldehyde, C9-aldehyde, C10-aldehyde, C11-aldehyde, C12-aldehyde, C13-aldehyde and C14-aldehyde.
[0205] The at least one type of α,β-unsaturated C6-C14 olefin is preferably selected from the group consisting of: hexene, heptenene, octene, nonene, decene, undecene, dodecene, tridecene, and tetradecene.
[0206] In a more preferred variant of the invention, component (a) of the aroma composition according to the invention is selected from the group consisting of decanoic acid and oleic acid, and / or component (b) is selected from the group consisting of 2E-decenal, 2E-undecenal and 2E,4E-decadienal, and / or component (c) is selected from the group consisting of 1-dodecene. These compounds primarily contribute to fatty / oily and / or smoky and / or roasted and / or caramel and / or animalic flavor profiles.
[0207] In another preferred variant, components (a), (b), and (c) are present in the aroma composition of the invention in a weight ratio of 4.5 to 6.5: 6.5 to 8.5: 4.5 to 6.5, preferably 5.0 to 6.0: 6.0 to 8.0: 5.0 to 6.0.
[0208] In a more preferred variant, the aroma composition of the present invention comprises the following components:
[0209] ≥150ppm, especially ≥230ppm of decanoic acid;
[0210] ≥250ppm, especially ≥350ppm of oleic acid;
[0211] ≥30ppm, especially ≥400ppm of 2E-decaldehyde; and
[0212] ≥50ppm, especially ≥120ppm, of 1-dodecene.
[0213] In a particularly preferred variant, the aroma composition of the present invention comprises the following components:
[0214] ≥200ppm, especially ≥230ppm of decanoic acid;
[0215] ≥250ppm, especially ≥350ppm of oleic acid;
[0216] ≥400ppm, especially ≥650ppm of 2E-decanoic acid;
[0217] ≥220ppm, especially ≥400ppm, of 2E-undecenal; and
[0218] ≥20ppm, especially ≥100ppm of 2E,4E-decadienal; and
[0219] ≥50ppm, especially ≥120ppm, of 1-dodecene.
[0220] As can be seen from Table 4, the aroma characteristics of the aroma composition with barbecue-like flavor characteristics according to the present invention are distinguished by the following contents: at least one type of straight-chain or branched, saturated or unsaturated aliphatic C8- to C20 monocarboxylic acid, such as decanoic acid and oleic acid; at least one type of α,β-unsaturated C6-C14 aldehyde, such as C6-aldehyde, C7-aldehyde, C8-aldehyde, 2E-heptenal, C9-aldehyde, 2E-oxenal, 2E-nonenal, 2E-decenal, 2E-undecenal, 2E,4E-decadienal and 8Z-heptadecenal; and at least one type of α,β-unsaturated C6-C14 olefin, such as 2E-hexene, 11-hexene, 1-heptene, 1-octene, 4E-decene, 1-dodecene, 1,3E-undecadien and 8Z-heptadecene.
[0221] In a preferred variant, the aroma composition is characterized by a barbecue-like flavor profile with a high concentration of decanoic acid, oleic acid, 2E-decenal, 2E-undecenal, 2E,4E-decadienal, and 1-dodecene, as described above. The concentrations of the aforementioned aldehydes and olefins in this aroma composition are significantly higher by at least 10 times compared to the aroma composition according to WO 2019 / 141357A1, as can be seen from Table 4. This also applies to the concentrations of decanoic acid and oleic acid, where the multiple is at least 2.
[0222] The aroma compositions produced using this invention are very strong and unique. Due to their distinctive characteristics and barbecue flavor features, another aspect of the invention relates to the use of this aroma composition to provide or enhance a barbecue flavor in food, food supplements, or animal feed, and particularly to impart fatty / oily and / or smoky and / or roasted and / or caramelized and / or animal flavor profiles, and to simultaneously suppress and / or reduce waxy flavor profiles, and / or for use in the preparation of food, food supplements, or animal feed.
[0223] This aroma composition can be used alone or in combination with other flavorings to obtain blended products. The aroma composition of this invention can also be used with suitable liquid or solid carriers (such as maltodextrin, starch, or other carriers described in detail above), or as a flavoring agent with one or more other suitable food additives. The flavoring agent can be in liquid, solid, sauce, cream, paste, or powder form.
[0224] The aroma composition according to the invention, or a mixture or flavoring containing the aroma composition, can then be applied to meat, poultry, fish / seafood and / or other foods, including but not limited to dairy products, vegetables, fried, sautéed, baked, microwaved, grilled, barbecued or snack foods, where it is necessary to impart or enhance a barbecue flavor.
[0225] Therefore, another aspect of the present invention relates to food, food supplements, or animal feed comprising the aroma composition according to the present invention. The food is selected from, but not limited to, meat, poultry, fish / seafood, dairy products, vegetables, fried, sautéed, baked, microwaved, grilled, barbecued, or snack foods. The aroma composition, or a mixture containing the aroma composition, or a flavoring agent is added to the food, food supplement, or animal feed at a concentration sufficient to impart a barbecue-like flavor to the aforementioned product. In particular, the aroma composition, or a mixture containing the aroma composition, is added to the aforementioned consumer product in an amount of 0.01% to 0.3% by weight, preferably 0.02% to 0.2% by weight, and most preferably 0.1% by weight, based on the total weight of the formulation.
[0226] Finally, the present invention relates to an apparatus for producing an aroma composition having a barbecue-like flavor profile, the apparatus having a reactor 1 comprising:
[0227] (i) a reservoir 2 for vegetable oil or animal oil or fat or a mixture thereof, a pump 3, and a device suitable for heating the vegetable oil or animal oil.
[0228] 4. A heater for producing a heated oil flow from oil or fat or a mixture thereof;
[0229] (ii) An atomizing device, preferably nozzle 6, which is adapted to atomize the heated oil stream so as to atomize the oil...
[0230] The stream is broken down into a liquid oil phase and an aerosol containing an aroma composition with barbecue-like flavor characteristics;
[0231] (iii) Optionally, inlet 7, the inlet being adapted to inject fluid or gas near the nozzle outlet or to apply fluid or gas near the nozzle outlet.
[0232] Add vacuum;
[0233] (iv) Second pipeline 9, which is adapted to discharge the aerosol containing the barbecue flavor;
[0234] (v) Third pipeline 10, which is adapted to return the liquid oil phase to the reactor;
[0235] (vi) Container 11, which is adapted to collect the aerosol; and
[0236] (vii) Collector 12, which is adapted to collect the liquid oil phase.
[0237] In a preferred variant of the device, heater 4 is an induction heater. This provides a smoother heating curve.
[0238] In a more preferred variant of the device, nozzle 6 is a venturi nozzle, an example of which is shown in Figure 6 Described in the text.
[0239] Additional preferred variations and configurations of the device according to the invention are described in conjunction with the method according to the invention.
[0240] List of reference numerals in the attached diagram:
[0241] 1. Reactor
[0242] 2. Storage container
[0243] 3 pumps
[0244] 4 heaters
[0245] 5 First pipeline
[0246] 6 nozzles
[0247] 7 entrances
[0248] 8 Vacuum Control Unit
[0249] 9 Second pipeline
[0250] 10 Third Pipeline
[0251] 11 Containers
[0252] 12 Collection Containers
[0253] 13. Expel air / partial vacuum
[0254] Example 1: Characterization of the reaction products
[0255] Using 100 ppm 2-nonanol as an internal standard, each 0.5 g product sample (sunflower oil with high oleic acid content) was extracted in 2 g of water by SBSE (stirred rod adsorption extraction) for 1 hour, and analyzed by GS / MS.
[0256] One sample relates to an aroma composition prepared according to the invention, wherein the liquid oil phase is recycled twice; another sample relates to an aroma composition prepared according to the invention, wherein the liquid oil phase is recycled four times; and yet another sample relates to an aroma composition prepared according to the invention, wherein the liquid oil phase is recycled six times.
[0257] For comparison, samples of aroma compositions prepared using the same raw materials according to the method of WO 2019 / 141357 A1 were prepared.
[0258] instrument:
[0259]
[0260] TDU_40_3_230_S10_150℃M:
[0261] 40℃ (1min isotherm) – 3℃ / min – 230℃ (25min isotherm)
[0262] Flow split: 1:10 (TDU maximum temperature: 150℃)
[0263] GC:
[0264] Oven temperature
[0265] (Initial) -> 40℃
[0266] program
[0267] #1 Rate 3℃ / min
[0268] #1 Value: 230℃
[0269] #1 Holding time: 30 minutes
[0270] Former PTV entrance He
[0271]
[0272]
[0273]
[0274] Pre-detector FID
[0275]
[0276] MSD transmission pipeline
[0277] temperature
[0278] (Initial) 280℃
[0279] FID signal
[0280] Signal #1 Front-end signal (FID)
[0281] Data rate 20Hz
[0282] GERSTEL CIS
[0283] Temperature program:
[0284] Initial temperature -20℃
[0285] Equilibrium time: 1.00 min
[0286] Initial time: 0.10 min
[0287] Slope 1
[0288] Rate 12.00℃ / s
[0289] Finishing temperature 250℃
[0290] Hold time: 10.00 min
[0291] GERSTEL TDU
[0292] Temperature program:
[0293] Initial temperature 30℃
[0294] Delay time: 1.00 min
[0295] Initial time: 0.00 min
[0296] Slope 1
[0297] Rate 1 60.0℃ / min
[0298] End temperature 1 150℃
[0299] Holding time 1 8.00 min
[0300] TDU Settings
[0301]
[0302] Basic Information
[0303] Scan parameters:
[0304] Low quality 25
[0305] High quality 370
[0306] MSZones:
[0307] Mass spectrometry source 230℃, maximum 250℃
[0308] Mass spectrometer quadrupole 150℃, maximum 200℃
[0309] The results of gas chromatography are shown in Table 4 below.
[0310] Table 4:
[0311]
[0312]
[0313]
[0314]
[0315]
[0316]
[0317]
[0318]
[0319]
[0320] Example 2: Characterization of the reaction products
[0321] Using 100 ppm 2-nonanol as an internal standard, 0.5 g of rapeseed oil was extracted in 2 g of water by SBSE (stirred rod adsorption extraction) for 1 hour, and analyzed by GS / MS.
[0322] The sample relates to an aroma composition prepared according to the present invention, wherein the liquid oil phase is recycled four times.
[0323] Sample analysis was performed under the same MS / GC analysis conditions as described in Example 1.
[0324] The results of gas chromatography are shown in Table 5 below and compared with those of the high-oleic sunflower oil sample according to Example 1. Table 5 is only an excerpt of the main components of the flavor profile, and does not include all components of the flavor profile.
[0325] Table 5:
[0326]
[0327]
[0328]
[0329]
[0330] Table 5 shows that the barbecue flavor characteristics of rapeseed oil are characterized by significant contents of decanoic acid, oleic acid, 2E-decenal, and 1-dodecene (despite differences in the fatty acid composition of the starting materials). This results in a barbecue flavor profile dominated by barbecue aroma, characterized by an extremely high proportion of fatty / oily and / or smoky and / or roasted and / or caramelized and / or animalic aromas.
[0331] Example 3: Sensory Evaluation
[0332] Sensory evaluation was performed on samples of the aroma composition according to the present invention obtained in Example 1 (4 cycles).
[0333] For comparison, samples of aroma compositions prepared according to WO 2019 / 141357 A1, as obtained in Example 1, were used.
[0334] A panel of four experts (flavorists) evaluated and compared the odor and intensity of aroma compositions (0.1% in water) on a scale of 1 to 8. Sensory evaluation was conducted by placing 30 ml of the test solution in an 80 ml plastic cup.
[0335] The flavor profiles used as parameters are: fatty / oily, soapy, waxy, caramel, roasted, phenolic, smoky, animalic, green, and impact.
[0336] from Figure 7 As can be seen from the spider diagram, the aroma composition according to the present invention has a higher influence, and the fatty / oily and / or smoky and / or roasted and / or caramel and / or animalic flavor profiles are significantly enhanced, while the waxy flavor profiles are suppressed compared to the aroma composition according to the prior art WO 2019 / 141357.
Claims
1. A method for preparing an aroma composition having a barbecue-like flavor profile, the method comprising or consisting of the following steps in sequence: (a) Provide vegetable oils or animal oils or fats or mixtures thereof; (b) In the absence of air or oxygen in the reaction zone, the product of step (a) is transferred to the reactor and heated to 310°C to 400°C and a pressure in the range of 2 bar to 6 bar to obtain an oil flow. (c) The oil stream is atomized by an atomizing device, thereby breaking the oil stream into a liquid oil phase and an aerosol containing an aroma composition with barbecue-like flavor characteristics. (d) Transfer the aerosol containing the aroma to a second pipeline and transfer the liquid oil phase to a third pipeline; (e) The aerosol containing the aroma is discharged by collecting the aerosol or adsorbing the aerosol onto a solid or liquid carrier; as well as (f) Optionally, the liquid oil phase from step (d) is returned to the reactor.
2. The method according to claim 1, wherein in step (b), the product of step (a) is heated to a temperature in the range of 350°C to 380°C.
3. The method according to claim 1, wherein the atomizing device is a nozzle.
4. The method according to claim 1, wherein in step (b) the product of step (a) is heated to a temperature in the range of 360°C to 370°C and / or a pressure in the range of 3 bar to 4 bar and / or heated for 10 seconds to 30 seconds.
5. The method according to any one of claims 1 to 4, wherein the method comprises 2 to 5 cycles.
6. The method of claim 5, wherein the method comprises 3 to 4 cycles.
7. The method according to any one of claims 1 to 4, wherein step (b) is performed without purging air.
8. The method according to any one of claims 1 to 4, wherein the atomization step is performed by flash evaporation and / or by a venturi nozzle.
9. The method according to any one of claims 1 to 4, wherein step (c) further comprises injecting fluid or gas near the nozzle outlet, or applying a vacuum near the nozzle outlet at a pressure in the range of 200 mbar to 800 mbar.
10. The method according to any one of claims 1 to 4, wherein the vegetable oil or animal oil or fat in step (a) is selected from the group consisting of: unsaturated, saturated or partially saturated palm oil, palm kernel oil, soybean oil, sunflower oil, peanut oil, olive oil, rapeseed oil, grapeseed oil, canola oil, corn oil, coconut oil, sesame oil, poppy seed oil, safflower oil, pumpkin seed oil, rice bran oil, almond oil, pecan oil, macadamia nut oil, cottonseed oil, flaxseed oil, pork fat, beef fat, mutton fat, bacon fat, chicken fat, turkey fat, butter, or a mixture of two or more of these oils and / or fats.
11. An aroma composition that can be obtained by means of any one of claims 1 to 10, optionally in combination with a solid or liquid carrier and / or other suitable food additives.
12. The aroma composition according to claim 11, wherein the aroma composition comprises: (a) at least one type of straight-chain or branched, saturated or unsaturated aliphatic C8-C20 monocarboxylic acid; (b) at least one type of α,β-unsaturated C6-C14 aldehyde; and (c) At least one type of α,β-unsaturated C6-C14 olefin.
13. The aroma composition according to claim 12, wherein the aroma composition comprises: (a) Two types of straight-chain or branched, saturated or unsaturated aliphatic C8-C20 monocarboxylic acids; (b) Two types of α,β-unsaturated C6-C14 aldehydes; and (c) Two types of α,β-unsaturated C6-C14 alkenes.
14. The aroma composition according to any one of claims 11 to 13, wherein: Component (a) is selected from the group consisting of decanoic acid and oleic acid; and / or Component (b) is selected from the group consisting of 2E-decanoal, 2E-undecanoal and 2E,4E-decadienal; and / or Component (c) is selected from the group consisting of 1-dodecene.
15. The aroma composition according to claim 14, wherein the components (a), (b), and (c) are present in a weight ratio of 4.5 to 6.5: 6.5 to 8.5: 4.5 to 6.
5.
16. The aroma composition according to claim 14, wherein the aroma composition comprises the following components: ≥150ppm of decanoic acid; ≥250ppm oleic acid; ≥30ppm of 2E-decenal; and ≥50 ppm of 1-dodecene.
17. The aroma composition according to claim 16, wherein the aroma composition comprises the following components: ≥230ppm of decanoic acid; ≥350ppm oleic acid; ≥400ppm of 2E-decenal; and ≥120ppm of 1-dodecene.
18. The aroma composition according to any one of claims 11 to 17 is used to provide or enhance fatty / oily and / or smoked and / or roasted and / or caramelized and / or animal flavors in food, food supplements or animal feed and to simultaneously suppress and / or reduce waxy flavors, and / or for use in the preparation of food, food supplements or animal feed.
19. A food, food supplement, or animal feed comprising the aroma composition according to any one of claims 11 to 17.
Citation Information
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