Set-up for the preparation of a powder

Abstract

This invention relates to a method for manufacturing spray-dried powder. A solvent is used during this method. The method is carried out in multiple steps such that the emulsion mass ratio is low when the solvent is first removed. Preferred solvents are isopropyl acetate and ethyl acetate. This invention also relates to an setup for carrying out the method of this invention on an industrial scale.

Description

[Technical Field]

[0001] Field of the Invention This invention relates to the manufacture of spray-dried powders that, although containing fat-soluble compounds, are still water-dispersible. A typical fat-soluble compound is β-carotene. Such powders can be used for coloring food and beverages. [Previous Technology]

[0002] Background of the Invention Edible colorants are needed to color food and beverages. Many edible colorants are fat-soluble. To make fat-soluble colorants water-dispersible, they need to be sealed with edible emulsifiers. Well-known edible emulsifiers include gelatin and modified starch.

[0003] Aqueous dispersible powders containing fat-soluble compounds can be manufactured by spray drying. For this purpose, a dispersion containing (i) water and (ii) particles is spray-dried. The particles of the dispersion contain fat-soluble compounds in their core, surrounded by an edible emulsifier. For suitability for coloring food and beverages, the particles must be extremely small. Typically, the particles have a particle size of less than 1 µm.

[0004] Dispersions suitable for spray drying can be manufactured in different ways.

[0005] EP 0 937 412 B1 discloses a method for preparing powdered carotene, retinoids, or natural colorants, wherein the active ingredient is finely pulverized, the method comprising the following steps: a) forming a suspension of the active ingredient in a water-immiscible organic solvent, optionally containing an antioxidant and / or an oil, such as dimethyl carbonate, ethyl formate, ethyl acetate or isopropyl acetate, methyl tributyl ether or dichloromethane; b) feeding the suspension of step a) into a heat exchanger and heating the suspension to 100°C to 180°C, wherein the residence time in the heat exchanger is less than 5 seconds; c) rapidly mixing the solution of step b) with an aqueous solution of a swellable colloid optionally containing a stabilizer at a temperature in the range of 20 to 100°C; d) removing the organic solvent; and e) converting the dispersion of step d) into a powdered preparation.

[0006] In Example 1 of EP 0 937 412 B1, a powder containing gelatin and having a carotene content of 11.6% was obtained. Although this powder is applicable, it needs to be a gelatin-based powder with a high carotene content. In order to obtain a high carotene content in the powder, the spray-dried dispersion must also have a high carotene content.

[0007] The problem to be solved by the present invention is to provide an aqueous dispersion that can be converted into a water-dispersible powder (e.g., by spray drying) and / or has a high content of at least one fat-soluble compound, such as a fat-soluble colorant.

[0008] The manufacture of this dispersion is a technical challenge. Ideally, the dispersion is of such high quality that when filtered through 2 g of Hyflo Super Cel® filter paper (Whatman 1001-070, grade 1, with a mesopore size of 7.0 μm), there is virtually no filtration residue.

[0009] Therefore, the more specific problem to be solved by the present invention is to provide a method for the industrial manufacture of an aqueous dispersion, wherein: - when the dispersion is filtered on 2 g of Hyflo Super Cel® on filter paper (Whatman 1001-070, grade 1, with an intermediate pore size of 7.0 μm), it has a filtration residue of less than 4% by weight of the total weight of the dispersion, and - can be converted into an aqueous dispersible powder by spray drying, and / or - has a high content of at least one fat-soluble compound (e.g., a fat-soluble colorant). [Summary of the Invention]

[0010] Summary of the Invention This invention relates to a powder containing at least one fat-soluble compound. The powder is preferably water-dispersible and preferably contains a large amount of at least one fat-soluble compound.

[0011] In order to manufacture the powder of the present invention, the aqueous dispersion is spray-dried. In order to obtain high-quality powder, the spray-dried dispersion must have low filtration residue when filtered through 2 g of Hyflo Super Cel® on filter paper (Whatman 1001-070, grade 1, with an intermediate pore size of 7.0 μm).

[0012] The spray-dried dispersion is obtained by removing the solvent of an intermediate composition in an evaporator. The intermediate composition comprises water and particles, wherein the particles have a core and a shell, and wherein the shell contains at least one emulsifier, and wherein the core contains at least one fat-soluble compound and a solvent, characterized in that the particle-solvent distribution of the particles in the composition is bimodal.

[0013] The emulsifier of the present invention is preferably a polymer and even more preferably a colloid, such as a hydrophilic colloid. Preferably, the emulsifier of the present invention is modified starch (such as modified food starch) or gelatin (such as fish gelatin). The preferred modified food starch is octenyl succinate starch.

[0014] The intermediate composition of the present invention may contain only one type of solvent or a mixture of different types of solvents. The objective of the evaporation step is to remove (multiple) solvents from the core of the particles. During solvent evaporation, only a portion of the water in the dispersion relevant to the applicable VLE (vapor-liquid equilibrium) is evaporated. Therefore, the resulting dispersion is a liquid. In the context of the present invention, water is not considered a solvent.

[0015] In one preferred embodiment of the invention, the fat-soluble compound is solid at a temperature of 25°C. An example of such a compound is β-carotene. When using such a compound, the core of the particles may further contain at least one oil, such as a vegetable oil. The oil is not removed during the evaporation step, and therefore the oil is not considered a solvent.

[0016] This invention also relates to the industrial manufacturing of a dispersion to be spray-dried. For this purpose, suitable setups are disclosed. The setup of this invention is for spray-drying a dispersion. Therefore, the setup of this invention preferably also includes equipment for spray drying, such as a spray drying tower.

[0017] The present invention comprises an evaporator (1), a mixing unit (2), a container (3), a container (4) and a mixing unit (5), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b) and a liquid outlet (1c), and wherein the evaporator (1), the mixing unit (2), the container (3) and the mixing unit (5) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2) and from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1), characterized in that the container (4) is configured such that a liquid composition can be fed from the container (4) to the mixing unit (2) and to the mixing unit (5).

Implementation Method

[0031] A detailed description of the preferred embodiment is that a powder can be obtained, for example, by spray drying an aqueous dispersion containing particles. Other methods for converting aqueous dispersions into powders are also known.

[0032] In the prior art method, a dispersion to be spray-dried is obtained by removing the solvent from the emulsion (see Figure 1). If the emulsion mass ratio is too high, the quality of the dispersion to be spray-dried is poor. Poor quality means that the obtained spray-dried powder is not completely water-dispersible, i.e., it contains some of the dynamic floats or sediments in the beverage. Therefore, it is difficult or even impossible to manufacture powders containing a very large amount of at least one fat-soluble compound using the prior art solvent method.

[0033] In the method of the present invention, a dispersion to be spray-dried is obtained by removing solvent from a specific composition (hereinafter referred to as the "intermediate composition"; see Figures 4 and 5). Unexpectedly, the resulting dispersion exhibits excellent quality, even when the intermediate composition is highly concentrated. Therefore, it is possible to manufacture powders and / or dispersions containing a large amount of at least one fat-soluble compound, even using low-efficiency solvents such as ethyl acetate or isopropyl acetate. Low efficiency means requiring a relatively large amount of solvent at a relatively high temperature to dissolve fat-soluble colorants such as β-carotene or lycopene. Ethyl acetate and isopropyl acetate offer advantages such as lower cost and improved safety and sustainability. Limitations of prior art methods

[0034] The method used in the comparative example is illustrated in Figures 1 and 2. The core of the emulsion particles contains solvent. When the emulsion is heated in an evaporator, the solvent escapes / is removed from the core of the particles, i.e., the volume of the core decreases. Therefore, when the solvent is removed, the particles become smaller.

[0035] When using highly concentrated emulsions, the methods of the prior art fail.

[0036] Although we do not wish to be bound by any particular theory or mechanism, it is believed that when the core of the particles contains too much solvent, that is, when the internal phase is also large, the particles collapse during the emulsification step or in the evaporator.

[0037] A small amount of solvent can pass through the shell of the particle because the shell is slightly flexible: the emulsifier molecules forming the core temporarily separate to allow solvent molecules to pass through. Unfortunately, this mechanism fails when too many solvent molecules attempt to pass through the particle shell at the same time: this causes the particles to burst / collapse. The remaining collapsed particles then agglomerate or aggregate. Therefore, when the dispersion is filtered after the evaporation step, the filtration residue increases to an unacceptably high level. This hypothetical mechanism is shown in Figure 2.

[0038] When the critical emulsification mass ratio of the selected system is exceeded, the particles collapse during the emulsification step or the evaporation step. When using prior art methods, the critical emulsification mass ratio is exceeded relatively rapidly. This is illustrated in Figure 3 using a hypothetical illustrative system. Inventive Concept

[0039] The method of the present invention is shown in Figure 4: the emulsification step and the evaporation step are split into multiple steps. Therefore, particles with a large amount of solvent in the core are not formed during the method. The particles do not collapse during the emulsification or evaporation step. This mechanism is shown in Figure 5: only one part of the lipophilic compound is emulsified. During emulsification, particles containing a relatively small amount of solvent in the core are formed. This small amount of solvent can be removed by evaporation without causing the particles to collapse. Then the second part of the lipophilic compound is emulsified. Then, the solvent from the core of the newly formed particles is removed by evaporation. The old particles are stable enough to withstand the second emulsification / evaporation step. When using the setup of the present invention, the number of times the old particles must undergo another emulsification / evaporation step can be controlled. In the setup shown in Figures 7 and 8, the particles formed in the mixing unit (2) / evaporator (1) must undergo two other emulsification / evaporation steps, while the particles formed in the mixing unit (5) / evaporator (6) must only undergo one other emulsification / evaporation step.

[0040] Since the particles do not collapse when using the method of the present invention, a highly concentrated dispersion of a fat-soluble compound of excellent quality can be produced. Furthermore, if the highly concentrated dispersion is spray-dried, a highly concentrated powder is obtained.

[0041] In the method of the present invention, the emulsification step and the evaporation step are performed at least twice. Therefore, it is possible to perform the method of the present invention in a cyclic manner. If the method is performed in a cyclic manner, it cannot be ruled out that some particles must undergo significantly more than two other emulsification / evaporation steps. Therefore, using a configuration with multiple mixing units / evaporators is a more gradual / mild approach. Definition

[0042] In the context of this invention, "dispersion" may be an emulsion, i.e., the core of the particles may be a liquid. Alternatively, the dispersion may be a suspension, i.e., the core of the particles may be a solid. However, in one typical embodiment of this invention, the core of the dispersion comprises both liquid and solid compounds.

[0043] The "particles" of the dispersion are too small to be seen with the naked eye. In one preferred embodiment of the invention, the particles have an average size in the range of 50 to 1000 nm, more preferably 100 to 800 nm, and even more preferably 100 to 500 nm [average size measured cumulatively by photon correlation spectroscopy (Beckman Coulter N4 Plus submicron particle size analyzer)]. "Average size cumulatively" refers to the z-mean, preferably determined according to ISO 22412:2008. Despite having an oleophilic core, the particles are water-dispersible. This is achieved by using an emulsifier surrounding the core. This surrounding is called the shell of the particle. The core of the particle may or may not contain a solvent. If it contains a solvent, it may be only one solvent or a mixture of multiple solvents.

[0044] The "solvent" of this invention is an organic solvent, preferably having a boiling point of less than 120°C, more preferably less than 100°C, at 1013,25 hPa. Any organic solvent mentioned in EP 0 937 412 may be used, provided that the selected fat-soluble compound is at least partially soluble therein. Preferred solvents are water-immiscible or water-miscible organic solvents, such as dimethyl carbonate, ethyl formate, ethyl acetate or isopropyl acetate, methyl tributyl ether, and dichloromethane, with isopropyl acetate and ethyl acetate being particularly preferred. In the context of this invention, oil is not considered a solvent. Typically, oil has a boiling point of more than 120°C at 1013,25 hPa. In the context of this invention, water is also not considered a solvent.

[0045] The distribution function of a specific property quantitatively defines how the value of that property is distributed among particles in the entire population. In the context of this invention, the relevant property is the number of solvent molecules in the core of the particle. Therefore, in the context of this invention, "particle-solvent-distribution" refers to the number of particles present according to the number of solvent molecules in the core. The particle-solvent-distribution function P(S) is defined by P(S) = the number of particles in a population with S solvent molecules in the core, where the symbol S is a non-negative integer (i.e., ℕ0 = {0;1;2;3;4;…}). "Bimodal" means that two distinct peaks (local maxima) appear in the smoothed particle-solvent-distribution function P(S) as illustrated in Figure 9. Those skilled in this art are familiar with "smoothing". Smoothing allows important patterns to be captured in data while omitting noise or other fine-scale structures. Therefore, as a rough approximation, bimodal means that there are two types of particles: some particles contain many solvent molecules in the core, while other particles contain no solvent molecules or very few solvent molecules in the core.

[0046] The "intermediate composition" of the present invention is a composition comprising water and particles, wherein the particles have a core and a shell, and wherein the shell comprises at least one emulsifier, and wherein the core comprises at least one fat-soluble compound and a solvent, characterized in that the particle-solvent distribution of the particles in the composition is bimodal.

[0047] Therefore, roughly speaking, the intermediate composition comprises two types of particles, wherein the two types of particles differ from each other in the amount of solvent in the core. In one preferred embodiment of the invention, the core of one type of intermediate composition is substantially solvent-free, while the core of the other type of intermediate composition contains a significantly large number of solvent molecules. "Substantially solvent-free core" means that the core of the particles contains less than 10,000 ppm, preferably less than 100 ppm, and most preferably less than 10 ppm of solvent molecules (ppm = molar fraction). "A substantial number of solvent molecules" preferably means at least 5% solvent molecules, more preferably at least 40% solvent molecules, and most preferably at least 85% solvent molecules, based on the total number of molecules in the core of the particles.

[0048] A fat-soluble compound is understood to have water solubility of less than 5 g fat-soluble compound / L water at 20°C, preferably less than 2 g fat-soluble compound / L water at 20°C, and most preferably less than 1 g fat-soluble compound / L water at 20°C. Preferably, the "fat-soluble compound" is a fat-soluble colorant or a fat-soluble micronutrient, such as fat-soluble vitamins and fatty acids. In a more preferred embodiment of the invention, the fat-soluble compound is a carotenoid, retinoid, or natural colorant mentioned in paragraph

[0015] of EP 0 937 412 B1. In one or even a preferred embodiment of the present invention, the fat-soluble compound is β-carotene, lycopene, β-apo-4'-carotene aldehyde, β-apo-8'-carotene aldehyde, β-apo-12'-carotene aldehyde, β-apo-8'-carotene acid, astaxanthin, canthaxanthin, zeaxanthin cryptoxanthin, citrinin, lutein, saccharomycin aldehyde, saccharomycin ethyl ester, spirulinacin ethyl ester, ζ-carotene, or dehydrosaccharomycin. In the preferred embodiment of the present invention, the fat-soluble compound is β-carotene or lycopene.

[0049] Therefore, one embodiment of the present invention relates to a composition comprising water and particles, wherein the particles have a core and a shell, and wherein the shell comprises at least one emulsifier, and wherein the core comprises at least one fat-soluble compound and a solvent. The composition is characterized by a bimodal particle-solvent distribution of the particles, and is further characterized by the fact that the at least one fat-soluble compound is carotene, retinoids, and / or a colorant, and / or preferably β-carotene, lycopene, β-deco-4'-carotene aldehyde, β-deco-8'-carotene aldehyde, β-deco-12'-carotene aldehyde, β-deco-8'-carotene acid, astaxanthin, canthaxanthin, zeaxanthin cryptoxanthin, citrinin, lutein, saccharin aldehyde, saccharin ethyl ester, spirulina ethyl ester, ζ-carotene, dehydrosaccharin, annatto, saffron, crocin, capsicumin, capsicum rubigin, rubigin, violetin, and / or pinocembrin, carmine acid, curcumin, and / or a metal chelate of chlorophyll.

[0050] In the context of this invention, the term "lipophilic compound" refers to (a) at least one fat-soluble compound, (b) (multiple) solvents, and (c) an oil, if any. The lipophilic compound is supplied by a container (4) provided by the present invention (see below). The term "hydrophilic matrix" refers to (1) water, (2) at least one emulsifier, and (3) other water-soluble compounds, such as sugars, if any, present.

[0051] In the context of this invention, "emulsion mass ratio" refers to a composition comprising (i) a lipophilic compound (= a fat-soluble compound, a solvent, and an oil of choice) and (ii) a hydrophilic matrix and is calculated as follows:

[0052] Alternatively, the emulsification mass ratio can be expressed as a percentage:

[0053] When filtering dispersions after removing the solvent (and partially removing water, depending on the applicable vapor-liquid equilibrium), if the relative amount of lipophilic compounds in individual dispersions exceeds a certain threshold, the filtration residue increases significantly. In the context of this invention, this threshold is referred to as the "critical emulsification mass ratio" (see the hypothetical example in Figure 3). The value of the critical emulsification mass ratio of the system depends on the selected solvent, lipophilic compounds, and emulsifier. For systems containing ethyl acetate or isopropyl acetate, the critical emulsification mass ratio is lower than that of corresponding systems containing high-efficiency solvents such as dichloromethane.

[0054] Any of the colloids mentioned in paragraph

[0021] of EP 0 937 412 B1 can be used as an emulsifier. However, the preferred emulsifiers of the present invention are modified starch and gelatin. In particular, the modified starch is octenyl succinate starch ("OSA starch"), preferably as defined in WO 2013 / 144221. OSA starch is commercially available, for example, under the trademarks HiCap® or Capsul®. The next most preferred emulsifiers are colloids, such as gum arabic, gum arabic, guar gum, locust bean gum, carboxymethyl cellulose, and seaweed gum.

[0055] "Settings" refers to a way of configuring things. In one preferred embodiment of the invention, settings are devices. The device may be part of a device that includes other equipment such as a spray drying tower.

[0056] In the context of this invention, the terms "weight" and "mass" of the composition are used interchangeably. Method for manufacturing a dispersion

[0057] Figure 1 shows the method used in the comparative example. It is a linear method, that is, emulsifying everything in one step before removing the solvent. In this method, the mass ratio of the two compositions must be selected such that it does not exceed the critical emulsification mass ratio (see the hypothetical example in Figure 3).

[0058] In contrast, the method of the present invention is an iterative process: a solution comprising a solvent and at least one fat-soluble compound is added stepwise, and thus the critical emulsification mass ratio of the system is never exceeded. Between these steps, the solvent is removed by evaporation. When the solvent is removed in an evaporator (preferably at a pressure of less than 1500 mbar, more preferably less than 1000 mbar), a small amount of water (e.g., less than 1% by weight of the water in the composition) also evaporates. Complete removal of the solvent is desirable but not absolutely necessary; that is, removing 95%, preferably 98%, and most preferably 99% of the solvent molecules contained in each composition is sufficient. The resulting composition may contain 1000 to 15000 ppm or less of solvent. To further reduce the amount of solvent (e.g., to a residual solvent level of less than 10 ppm), an additional evaporation step (not shown in the figures) may be applied.

[0059] Figure 4 illustrates the general principle of the present invention. Therefore, the present invention relates to a method for preparing a powder comprising at least one fat-soluble compound, wherein the method comprises the following steps: a) providing a solution comprising at least one fat-soluble compound, at least one solvent, and optionally at least one oil; b) providing a composition comprising water and at least one emulsifier; c) rapidly mixing a portion of the solution from step a) with a portion of the solution from step b) at a temperature in the range of 20 to 100°C; d) removing the at least one solvent by heating the composition from step c); e) adding an additional portion of the composition from step a) and optionally step b) to the composition from step d) under vigorous stirring; f) preferably removing the solvent by heating the composition from step e) at a pressure of less than 1500 mbar.

[0060] In step e) of this method, the intermediate composition of the present invention is obtained.

[0061] The present invention also relates to a method comprising the following steps: a) providing a solution comprising at least one fat-soluble compound, at least one solvent, and optionally at least one oil; b) providing a composition comprising water and at least one emulsifier; c) rapidly mixing a portion of the solution of step a) with a portion of the solution of step b) at a temperature in the range of 20 to 100°C; d) removing the at least one solvent by heating the composition of step c); e) adding an additional portion of the composition of step a) and optionally step b) to the composition of step d) under vigorous stirring; f) preferably removing the solvent by heating the composition of step e) under a pressure of less than 1500 mbar; g) adding an additional portion of the composition of step a) to the composition of step f) under vigorous stirring; and h) at least partially removing the solvent by heating the composition of step g) under a pressure of less than 1500 mbar.

[0062] In steps e) and g) of this method, the intermediate composition of the present invention is obtained. Therefore, the present invention also relates to a method comprising the steps of: a) providing a composition comprising water and particles, wherein the particles have a core and a shell, wherein the shell comprises at least one emulsifier, and wherein the core comprises at least one fat-soluble compound and at least one solvent, characterized in that the particle-solvent distribution of the particles in the composition is bimodal; b) preferably removing at least partially the organic solvent by heating the composition of step a) at a pressure preferably less than 1500 mbar; c) optionally converting the dispersion of step b) into a powder.

[0063] In a preferred embodiment of the present invention, the intermediate composition of the present invention comprises water and particles, wherein the particles have a core and a shell, and wherein the shell comprises at least one modified starch and / or at least one gelatin, and wherein the core comprises at least one coloring agent, at least one solvent and optionally at least one edible oil, wherein the at least one coloring agent is preferably β-carotene and / or lycopene, wherein the at least one solvent is preferably ethyl acetate and / or isopropyl acetate, and wherein the at least one edible oil is preferably corn oil, characterized in that the particle-solvent distribution of the particles in the composition is bimodal.

[0064] Therefore, one preferred embodiment of the present invention relates to a method comprising the following steps: a) providing a composition comprising water and particles, wherein the particles have a core and a shell, and wherein the shell comprises at least one modified starch and / or at least one gelatin, and wherein the core comprises at least one colorant, at least one solvent and optionally at least one edible oil, wherein the at least one colorant is preferably β-carotene and / or lycopene, wherein the at least one solvent is preferably ethyl acetate and / or isopropyl acetate, and wherein the at least one edible oil is preferably corn oil, and characterized in that the particle-solvent distribution of the particles in the composition is bimodal; b) preferably removing at least partially the organic solvent by heating the composition of step a); and c) optionally converting the dispersion of step b) into a powder.

[0065] The intermediate composition may have a relatively high emulsification ratio because a portion of the fat-soluble compound and optionally at least one oil are encapsulated in particles that are already solvent-free. In one preferred embodiment of the invention, at least 10%, preferably at least 20%, and most preferably at least 30% of the particles of the intermediate composition have a substantially solvent-free core.

[0066] The acceptable emulsification ratio of the intermediate composition depends on the system selected. The following list provides an overview of preferred embodiments of the intermediate compositions of the present invention: Intermediate composition, comprising… Emulsification ratio of intermediate composition …water …and particles, wherein such particles have… and…. …core, containing …shell, containing β-carotene, edible oil and ethyl acetate At least one modified starch 5% to 25%, preferably 5% to 20%, and optimally 5% to 15%. β-carotene, edible oil and ethyl acetate At least one type of gelatin 5% to 60%, better 5% to 50%, and optimal 5% to 40%. β-carotene, edible oil, and isopropyl acetate At least one modified starch 5% to 55%, better 5% to 50%, and optimal 5% to 40%. β-carotene, edible oil, and isopropyl acetate At least one type of gelatin 5% to 60%, better 5% to 55%, and optimal 5% to 45%. Lycopene, edible oil and ethyl acetate At least one modified starch 5% to 40%, better 5% to 30%, and optimal 5% to 20%. Lycopene, edible oil and ethyl acetate At least one type of gelatin 5% to 60%, better 5% to 50%, and optimal 5% to 40%. Lycopene, edible oil and isopropyl acetate At least one modified starch 5% to 60%, better 5% to 50%, and optimal 5% to 40%. Lycopene, edible oil and isopropyl acetate At least one type of gelatin 5% to 35%, better 5% to 30%, and optimal 5% to 25%. Spray-dried powder

[0067] The spray-dried powder of the present invention is water-dispersible and contains a high content of at least one fat-soluble compound. "High" means that the same content of the same fat-soluble compound cannot be achieved using the same system / solvent when employing prior art manufacturing methods. The exact value of "high" depends on the chosen system / solvent. The highest content can be achieved if dichloromethane is used as the solvent and / or if gelatin is used as the emulsifier, provided that the manufacturing method of the present invention is used. The following list provides an overview of preferred embodiments of the spray-dried powder of the present invention. In these preferred embodiments, a colloid is used as the emulsifier, wherein OSA starch is preferably a modified starch and fish gelatin is preferably gelatin: Powder Number fat-soluble compounds Oil (Yes / No) emulsifier The amount of fat-soluble compounds is based on the total weight of the spray-dried composition. 1 beta-carotene yes At least one modified starch At least 10% by weight, preferably at least 20% by weight 2 beta-carotene yes At least one type of gelatin At least 15% by weight, preferably at least 35% by weight 3 Lycopene no At least one modified starch At least 15% by weight, preferably at least 25% by weight 4 Lycopene no At least one type of gelatin At least 15% by weight, preferably at least 40% by weight set up

[0068] This invention also relates to a setup, i.e., a way of configuring things. In a preferred embodiment, the setup of this invention is a device.

[0069] When using the method of the present invention, it is preferred to use the setup of the present invention. The method of the present invention requires at least two emulsification steps. Therefore, the setup of the present invention includes at least two mixing units (see mixing units (2) and (5) in FIG. 6). In a preferred embodiment, the setup of the present invention includes at least three mixing units (see mixing units (2), (5) and (7) in FIG. 7 and FIG. 8).

[0070] Typically, the method of the present invention also requires at least two evaporation steps. Therefore, the arrangement of the present invention preferably includes at least two evaporators (see evaporators (1) and (6) in FIG. 6). In a preferred embodiment, the arrangement of the present invention includes at least three evaporators (see evaporators (1), (6) and (8) in FIG. 7 and FIG. 8).

[0071] The arrangement of the present invention is for sealing a fat-soluble compound with at least one emulsifier, wherein the at least one emulsifier is preferably a colloid. By sealing the fat-soluble compound, the fat-soluble compound becomes water-dispersible. Once sealed, spray drying can begin. Therefore, the arrangement of the present invention may also optionally include at least one device for spray drying (not shown in the figures).

[0072] The present invention comprises an evaporator (1), a mixing unit (2), a container (3), a container (4), and a mixing unit (5), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c), and wherein the evaporator (1), the mixing unit (2), the container (3), and the mixing unit (5) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2) and from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1). The container (4) is configured such that the liquid composition can be fed from the container (4) to the mixing unit (2) and the mixing unit (5), wherein the container (4) is preferably connected to the mixing unit (5) by means of a connector (4a), and wherein the connector (4a) is preferably a pipe, pipe, channel, funnel, flow path, conduit or trough.

[0073] In a preferred embodiment, the present invention comprises an evaporator (1), a mixing unit (2), a container (3), a mixing unit (5), and an evaporator (6), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c), and wherein the evaporator (6) has a feed inlet (6a), a steam outlet (6b), and a liquid outlet (6c), and wherein the evaporator (1), mixing unit (2), container (3), mixing unit (5), and evaporator (6) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2), and fed from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1), and fed from the mixing unit (5) to the evaporator (6) via the feed inlet (6a) of the evaporator (6). The container (4) is configured such that the liquid composition can be fed from the container (4) to the mixing unit (2) and the mixing unit (5), wherein the container (4) is preferably connected to the mixing unit (5) by means of a connector (4a), and wherein the connector (4a) is preferably a pipe, pipe, channel, funnel, flow path, conduit or trough.

[0074] In an even more preferred embodiment, the present invention comprises an evaporator (1), a mixing unit (2), a container (3), a mixing unit (5), an evaporator (6), a mixing unit (7), and an evaporator (8). The evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c). The evaporator (6) has a feed inlet (6a), a steam outlet (6b), and a liquid outlet (6c). The evaporator (8) has a feed inlet (8a), a steam outlet (8b), and a liquid outlet (8c). The evaporator (1), mixing unit (2), container (3), mixing unit (5), evaporator (6), mixing unit (7), and evaporator (8) are configured such that a liquid composition can be fed from the container (3) to the mixing unit. In unit (2), the feed is fed from mixing unit (2) to evaporator (1) via feed inlet (1a) and from evaporator (1) to mixing unit (5) via liquid outlet (1c), and from mixing unit (5) to evaporator (6) via feed inlet (6a) and from evaporator (6) to mixing unit (7) via liquid outlet (6c) and from mixing unit (7) to evaporator (8) via feed inlet (8a). The container (4) is configured such that the liquid composition can be fed from the container (4) into the mixing unit (2) and into the mixing unit (5), wherein the container (4) is preferably connected to the mixing unit (5) by means of a connector (4a), and / or wherein the container (4) is preferably connected to the mixing unit (7) by means of a connector (4b), and wherein the connector (4a) and / or the connector (4b) is preferably a pipe, pipe, channel, funnel, flow path, conduit or trough.

[0075] Preferably, the arrangement of the present invention is suitable for manufacturing powder on an industrial scale, i.e., manufacturing large quantities of powder. Therefore, the container (3) and / or the container (4) are preferably able to hold a volume of at least 100 liters, more preferably at least 500 liters, and most preferably at least 3000 liters. For the same reason, the connector (4a) and / or the connector (4b) preferably have a length of at least 2 meters, more preferably at least 10 meters, and most preferably at least 100 meters. Typically, the connector (4a) is connected to the inlet (5a) of the mixing unit (5). Similarly, the connector (4b) is typically connected to the inlet (7a) of the mixing unit (7).

[0076] Typically, the flow rate from container (4) to mixing unit (2), to mixing unit (5), and / or to mixing unit (7) needs to be adjustable. Therefore, the arrangement of the present invention preferably includes a component for controlling the flow from container (4) to mixing unit (2), to mixing unit (5), and / or to mixing unit (7). This component may be a pump.

[0077] Typically, the flow rate from the container (3) to the mixing unit (2) also needs to be adjustable. Therefore, the arrangement of the present invention preferably includes a component for controlling the flow from the container (3) to the mixing unit (2), wherein the container (3) preferably has a pump for controlling the flow from the container (3) to the mixing unit (2).

[0078] Therefore, one preferred embodiment of the present invention relates to an arrangement comprising an evaporator (1), a mixing unit (2), a container (3), a container (4), and a mixing unit (5), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c), and wherein the evaporator (1), the mixing unit (2), the container (3), and the mixing unit (5) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2) and from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1). The container (4) is configured such that the liquid composition can be fed from the container (4) to the mixing unit (2) and to the mixing unit (5), and the arrangement includes components for controlling the flow from the container (4) to the mixing unit (2) and to the mixing unit (5), and the arrangement preferably includes a pump for controlling the flow from the container (4) to the mixing unit (2) and / or the arrangement preferably includes a pump for controlling the flow from the container (4) to the mixing unit (5), and / or the arrangement includes components for controlling the flow from the container (3) to the mixing unit (2), and the container (3) preferably has a pump for controlling the flow from the container (3) to the mixing unit (2).

[0079] In an even more preferred embodiment, the present invention comprises an evaporator (1), a mixing unit (2), a container (3), a mixing unit (5), an evaporator (6), a mixing unit (7), and an evaporator (8), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c), and wherein the evaporator (6) has a feed inlet (6a), a steam outlet (6b), and a liquid outlet (6c), and wherein the evaporator (8) has a feed inlet (8a), a steam outlet (8b), and a liquid outlet (8c), and wherein the evaporator (1), the mixing unit (2), the container (3), the mixing unit (5), and the evaporator (6) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2), and via The feed is fed from the mixing unit (2) to the evaporator (1) through the feed inlet (1a) and from the evaporator (1) to the mixing unit (5) through the liquid outlet (1c) of the evaporator (1); and from the mixing unit (5) to the evaporator (6) through the feed inlet (6a) of the evaporator (6); and from the evaporator (6) to the mixing unit (7) through the liquid outlet (6c) of the evaporator (6) and from the mixing unit (7) to the evaporator (8) through the feed inlet (8a) of the evaporator (8). The container (4) is configured such that the liquid composition can be fed from the container (4) to the mixing unit (2) and to the mixing unit (5), and the arrangement includes components for controlling the flow from the container (4) to the mixing unit (2) and to the mixing unit (5), and the arrangement preferably includes a pump for controlling the flow from the container (4) to the mixing unit (2), to the mixing unit (5) and / or to the mixing unit (7), and / or the arrangement includes components for controlling the flow from the container (3) to the mixing unit (2), and the container (3) preferably has a pump for controlling the flow from the container (3) to the mixing unit (2).

[0080] In the above embodiments, the mixing unit (2), mixing unit (5) and / or mixing unit (7) are suitable for manufacturing emulsions. For this purpose, high shear force is required. Therefore, such mixing units are preferably homogenizing devices, such as high-pressure homogenizers (e.g., having a pressure drop of at least 50 bar, preferably 200 to 500 bar, and / or an orifice diameter of less than 1000 µm, preferably less than 500 µm and most preferably less than 300 µm), colloid mills, nozzles (e.g., nozzle diameter of 0.1 mm to 0.5 mm, preferably 0.2 mm to 0.3 mm), rotor-stator homogenizers (e.g., allowing a rotor speed of at least 3000 rpm, preferably at least 4000 rpm and most preferably at least 5000 rpm; rpm = revolutions per minute) or combinations of the aforementioned equipment.

[0081] In the above embodiments, the evaporator (1), evaporator (6) and / or evaporator (8) may be a vertical evaporator, a thin-film evaporator, a flash vessel, or any other type of evaporator that can be used to remove organic solvents. In a preferred embodiment, the evaporators are thin-film evaporators. Most preferably, the evaporators are fine-film evaporators.

[0082] When performing the method of the present invention, the container (4) typically holds a solution comprising at least one fat-soluble compound, at least one solvent, and optionally at least one oil. In a preferred embodiment, the solution is held in more than one container. In this preferred embodiment, the setup of the present invention includes a container (4'), a container (4''), and optionally a container (4''').

[0083] Therefore, the present invention also relates to an arrangement comprising an evaporator (1), a mixing unit (2), a container (3), a mixing unit (5), and an evaporator (6), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c), and wherein the evaporator (6) has a feed inlet (6a), a steam outlet (6b), and a liquid outlet (6c), and wherein the evaporator (1), the mixing unit (2), the container (3), the mixing unit (5), and the evaporator (6) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2), and fed from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1), and fed from the mixing unit (5) to the evaporator (6) via the feed inlet (6a) of the evaporator (6). The feature is that the arrangement further includes a container (4') and a container (4''), wherein the container (4') is configured such that the liquid composition can be fed from the container (4') into the mixing unit (2), and / or wherein the container (4'') is configured such that the liquid composition can be fed from the container (4'') into the mixing unit (5).

[0084] Another preferred embodiment relates to the arrangement of the present invention, which includes an evaporator (1), a mixing unit (2), a container (3), a mixing unit (5), an evaporator (6), a mixing unit (7), and an evaporator (8), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c), and wherein the evaporator (6) has a feed inlet (6a), a steam outlet (6b), and a liquid outlet (6c), and wherein the evaporator (8) has a feed inlet (8a), a steam outlet (8b), and a liquid outlet (8c), and wherein the evaporator (1), the mixing unit (2), the container (3), the mixing unit (5), and the evaporator (6) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2), and via The feed is fed from the mixing unit (2) to the evaporator (1) through the feed inlet (1a) and from the evaporator (1) to the mixing unit (5) through the liquid outlet (1c) of the evaporator (1); and from the mixing unit (5) to the evaporator (6) through the feed inlet (6a) of the evaporator (6); and from the evaporator (6) to the mixing unit (7) through the liquid outlet (6c) of the evaporator (6) and from the mixing unit (7) to the evaporator (8) through the feed inlet (8a) of the evaporator (8). The container (4) is configured such that the liquid composition can be fed from the container (4) into the mixing unit (2) and into the mixing unit (5), and is characterized in that the arrangement further comprises containers (4'), (4'') and (4'''), wherein the container (4') is configured such that the liquid composition can be fed from the container (4') into the mixing unit (2), and / or wherein the container (4'') is configured such that the liquid composition can be fed from the container (4'') into the mixing unit (5) and / or wherein the container (4''') is configured such that the liquid composition can be fed from the container (4''') into the mixing unit (7).

[0085] In a second preferred embodiment of the invention, the arrangement also includes equipment for spray drying, such as a spray drying tower. This equipment may be directly or indirectly connected to the liquid outlet of one of the evaporators. Preferred Embodiment

[0086] 1. Use of a device for sealing a fat-soluble compound, the device comprising an evaporator (1), a mixing unit (2), a container (3), a container (4), and a mixing unit (5), wherein the evaporator (1) has a feed inlet (1a), a vapor outlet (1b), and a liquid outlet (1c), and wherein the evaporator (1), the mixing unit (2), the container (3), and the mixing unit (5) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2) and from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1), characterized in that the container (4) is configured such that a liquid composition can be fed from the container (4) to the mixing unit (2) and to the mixing unit (5).

[0087] 2. As used in Embodiment 1, wherein the arrangement includes components for controlling the flow from container (4) to mixing unit (2) and / or to mixing unit (5), and wherein the arrangement preferably includes a pump for controlling the flow from container (4) to mixing unit (2) and / or wherein the arrangement preferably includes a pump for controlling the flow from container (4) to mixing unit (5), and / or wherein the arrangement includes components for controlling the flow from container (3) to mixing unit (2), and wherein container (3) preferably has a pump for controlling the flow from container (3) to mixing unit (2).

[0088] 3. As used in Embodiment 1 or 2, wherein the container (4) is connected to the mixing unit (5) by means of a connector (4a), wherein the connector (4a) is preferably a pipe, a conduit, a channel, a funnel, a flow path, a conduit or a groove, and / or wherein the connector (4a) preferably has a length of at least 2 meters, more preferably at least 10 meters and most preferably at least 100 meters.

[0089] 4. As used in any of the embodiments of the preceding claims, wherein each of the containers (3) and (4) is capable of holding a volume of at least 100 liters, preferably at least 500 liters and most preferably at least 3000 liters.

[0090] 5. Use of a device for sealing a fat-soluble compound, the device comprising an evaporator (1), a mixing unit (2), a container (3), a mixing unit (5), and an evaporator (6), The evaporator (1) has a feed inlet (1a), a steam outlet (1b) and a liquid outlet (1c), and the evaporator (6) has a feed inlet (6a), a steam outlet (6b) and a liquid outlet (6c). The evaporator (1), mixing unit (2), container (3), mixing unit (5) and evaporator (6) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2), and from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1), and from the mixing unit (5) to the evaporator (6) via the feed inlet (6a) of the evaporator (6). The feature is that the configuration is as described in any of the preceding claims, or the configuration further comprises a container (4') and a container (4''), wherein the container (4') is configured such that a liquid composition can be fed from the container (4') into the mixing unit (2), and / or wherein the container (4'') is configured such that a liquid composition can be fed from the container (4'') into the mixing unit (5).

[0091] 6. As used in Example 5, the arrangement further includes a mixing unit (7), wherein the mixing unit (7) is configured such that a liquid composition can be fed from the evaporator (6) to the mixing unit (7) via a liquid outlet (6c).

[0092] 7. As used in Example 6, the arrangement further includes an evaporator (8) having a feed inlet (8a), a steam outlet (8b) and a liquid outlet (8c), wherein the evaporator (8) is configured such that a liquid composition can be fed from the mixing unit (7) into the evaporator (8) via the feed inlet (8a).

[0093] 8. As in any of the foregoing embodiments, wherein the mixing unit (2), mixing unit (5) and / or mixing unit (7) is a homogenizer device and wherein the homogenizer device is preferably a homogenizer having a pressure drop of at least 50 bar, a colloid mill, a nozzle, a rotor-stator or a combination thereof.

[0094] 9. As used in any of the foregoing embodiments, wherein the evaporator (1), evaporator (6) and / or evaporator (8) is adapted to remove an organic solvent and / or to be a vertical evaporator, a thin-film evaporator or a flash evaporator.

[0095] 10. As used in any of the foregoing embodiments, the arrangement further includes equipment for spray drying, such as a spray drying tower.

[0096] 11. As used in any of the foregoing embodiments, wherein the fat-soluble compound is preferably an edible coloring agent, such as β-carotene or lycopene.

[0097] 12. As used in Example 11, wherein an emulsifier is used to seal the fat-soluble compound, and wherein the emulsifier is preferably a polymer, more preferably a colloid, and most preferably a hydrophilic colloid. Example

[0098] The present invention is further illustrated by the following examples. These examples are not intended to limit the invention in any way. Example 1a

[0099] In Example 1a, the method concept shown in Figure 4 is being used.

[0100] In a controlled 2-liter container, 389 g of modified food starch (commercially available HiCap®) was dissolved in 908 g of water at 76°C. Therefore, the 2-liter container contains approximately 1 liter of liquid.

[0101] In a separate controlled 2-liter container, 83.6 g of β-carotene, 10.3 g of dl-α-tocopherol, and 34.1 g of corn oil were dispersed in 422.0 g of ethyl acetate. The resulting dispersion was heated above its dissolution temperature to 121°C to produce a 15% by weight β-carotene solution. Thus, the 2-liter container contained approximately 0.5 liters of liquid.

[0102] The method concept shown in Figure 4 is followed, rather than mixing the two compositions in one step. Therefore, the emulsion mass ratio remains significantly below 30% at all times.

[0103] For example, in the mixing unit, an emulsification device is used. It consists of a rotor-stator followed by a royal blue orifice (280 µm in diameter). The rotor speed of the rotor-stator is 5000 rpm, the pressure drop inside the orifice of the mixing unit is 75 bar, and the temperature is 85°C.

[0104] To remove the solvent, the output of the mixing unit is fed into the evaporator via its feed inlet. Within the evaporator, a small portion of the solvent and water is removed. In this example, a fine thin-film evaporator is used at 72°C and 657 mbar.

[0105] The final dispersion contains 4.7% by weight of β-carotene, based on the total weight of the dispersion. The particles in the dispersion have an average particle size of 299 nm [average size measured cumulatively by photon correlation spectroscopy (Beckman Coulter N4 Plus submicron particle size analyzer)]. When this composition is spray-dried, it is expected to obtain a powder containing approximately 15.4% by weight of β-carotene based on the total weight of the powder. Example 1b (Comparative Example)

[0106] Repeat Example 1a. However, apply the method concept shown in Figure 1.

[0107] In a controlled 2-liter container, 389 g of modified food starch was dissolved in 908 g of water at 76°C. Therefore, the 2-liter container contained approximately 1 liter of liquid.

[0108] In a separately controlled 2-liter container, 83.6 g of β-carotene, 10.3 g of dl-α-tocopherol, and 34.1 g of corn oil were dispersed in 422 g of ethyl acetate. The resulting dispersion was heated above its dissolution temperature to 120°C to produce a 15% by weight β-carotene solution. Thus, the 2-liter container contained approximately 0.5 liters of liquid.

[0109] Once all the β-carotene has been dissolved, the lipophilic compound is added to the hydrophilic matrix phase upstream of the mixing unit.

[0110] For example, in the mixing unit, an emulsification device is used. The mixing unit is a rotor-stator followed by a royal blue orifice (280 µm in diameter). The rotor speed of the rotor-stator is 5000 rpm, the pressure drop inside the orifice of the mixing unit is 76 bar, and the temperature is 86°C.

[0111] The output of the mixing unit is an aqueous liquid containing only one type of particles: the core of these particles contains β-carotene, corn oil and solvent (=ethyl acetate), that is, the output of the mixing unit contains ethyl acetate.

[0112] To remove the solvent, the output of the mixing unit is then fed into the evaporator. Inside the evaporator, a small portion of the solvent and water is removed. In this example, a fine thin-film evaporator is used at 73°C and 600 mbar.

[0113] The final dispersion prepared by spray drying exits the liquid outlet of the evaporator and has a β-carotene content of 3.3% by weight, based on the total weight of the dispersion. The particles of the dispersion have an average particle size of 593 nm [average size measured cumulatively by photon correlation spectroscopy (Beckman Coulter N4 Plus submicron particle size analyzer)]. Example 2 (Measurement of Filtration Residue)

[0114] To check the quality of the final dispersion (i.e., the dispersion prepared for spray drying), the amount of filtration residue is determined by filtration. Low filtration residue indicates good quality, meaning it is suitable for spray drying. The following method is used:

[0115] The sample of the dispersion to be tested was used and the mass fraction (ws) of carotene in the sample was determined by UV / Vis.

[0116] Approximately 500 to 1500 mg of the sample (sample (ms)) was taken and the mass of carotene in the sample was calculated (ms × ws). The sample was then suspended in 250 ml of H2O (60°C), filtered through 2 g of Hyflo Super Cel® (CAS 68855-54-9, crystalline silica, bulk density: 300 kg / m3, available from Merck KGaA) on filter paper (Whatman 1001-070, grade 1, mesopore size 7.0 μm), and washed with 500 ml of H2O (60°C). The aqueous liquid was considered waste and was discharged.

[0117] The filtration residue was then washed with a filter containing approximately 100 ml of acetone and 40 ml of dichloromethane. Dichloromethane is an excellent solvent for carotenoids, and therefore, the resulting residual solution (RS) contained the filtration residue. The mass of carotenoids in the residual solution (mCaro.r) was then determined.

[0118] Next, the filtration residue is calculated as follows: FR = filtration residue as a percentage mCaro.r = mass of carotene in the residual solution (RS) mCaro.s = mass of carotene in the sample (ms×ws)

[0119] Any filtration residue less than 4% by weight of the total weight of the dispersion is desirable. Filtration residue exceeding 10% by weight of the total weight of the composition indicates the presence of improperly emulsified carotene.

[0120] The filtration residues of the dispersions in Example 1a and Comparative Example 1b have been measured. The results are shown in Table 1 below. Example 1a Comparison Example 1b Filter residue 1.4% by weight, based on the total weight of the dispersion. 53.2% by weight, based on the total weight of the dispersion. Table 1

[0121] Therefore, the method according to the invention reduces filtration residue by a factor of 35. This significant improvement is attributed to the emulsification mass ratio of the composition prior to evaporation. The emulsification mass ratio of Example 1b is slightly higher (about 30%) and is likely higher than the critical emulsification mass ratio of the system. Examples 3a and 3b (replacement of modified starch)

[0122] Examples 1a and 1b were repeated. However, a different type of modified starch (Capsul® instead of HiCap®) was used this time. In addition, no oil was used. A comparison of the compositions used in Examples 1a / 1b and Examples 3a / 3b is shown in Table 2 below. Example 1a / 1b Example 3a / 3b The composition in container (3) at the start of the method beta-carotene dl-α-tocopherol corn oil Ethyl acetate beta-carotene dl-α-tocopherol - Ethyl acetate The composition in container (4) at the start of the method HiCap® water Capsul® Glucidex® (glucose syrup) Sodium ascorbate water Table 2

[0123] In Example 3a, the method of the present invention is used. In Example 3b (=Comparative Example), the method of the prior art is used.

[0124] The filtration residues of the dispersions in Example 3a and Comparative Example 3b were measured as explained in Example 2. The results are shown in Table 3 below. Example 3a Comparative Example 3b Filter residue 3.9% by weight, based on the total weight of the dispersion. 54.9% by weight, based on the total weight of the dispersion. Table 3

[0125] The final dispersion obtained in Example 3a has a β-carotene content of 4.1% by weight, based on the total weight of the dispersion. The particles of the dispersion have an average particle size of 171 nm [average size measured cumulatively by photon correlation spectroscopy (Beckman Coulter N4 Plus submicron particle size analyzer)]. When this composition is spray-dried, it is expected to obtain a powder containing approximately 10.7% by weight of β-carotene based on the total weight of the powder.

[0126] Examples 3a and 3b confirm that filter residue can be reduced when using the method of the present invention. Examples 4a and 4b (Lycopene)

[0127] Examples 1a and 1b were repeated. However, this time a different type of fat-soluble compound (lycopene instead of β-carotene) was used. In addition, oil was not used. A comparison of the compositions used in Examples 1a / 1b and Examples 4a / 4b is shown in Table 4 below. Example 1a / 1b Example 4a / 4b The composition in container (3) at the start of the method beta-carotene dl-α-tocopherol corn oil Ethyl acetate Lycopene dl-α-tocopherol - Ethyl acetate The composition in container (4) at the start of the method HiCap® water Capsul® Glucidex® (glucose syrup) Sodium ascorbate water Table 4

[0128] In Example 4a, the method of the present invention is used. In Example 4b (=Comparative Example), the method of the prior art is used.

[0129] The filtration residues of the dispersions in Example 4a and Comparative Example 4b were measured as explained in Example 2. The results are shown in Table 5 below. Example 4a Comparison Example 4b Filter residue 3.6% by weight, based on the total weight of the dispersion. 43.8% by weight, based on the total weight of the dispersion. Table 5

[0130] Therefore, Examples 4a and 4b confirm that filter residue can be reduced when using the method of the present invention. Examples 5a and 5b (isopropyl acetate)

[0131] Examples 1a and 1b were repeated. However, a different type of solvent (isopropyl acetate instead of ethyl acetate) was used this time. A comparison of the compositions used in Examples 1a / 1b and Examples 5a / 5b is shown in Table 6 below. Example 1a / 1b Example 5a / 5b The composition in container (3) at the start of the method beta-carotene dl-α-tocopherol corn oil Ethyl acetate beta-carotene dl-α-tocopherol corn oil Isopropyl acetate The composition in container (4) at the start of the method HiCap® water HiCap® water Table 6

[0132] In Example 5a, the method of the present invention is used. In Example 5b (=Comparative Example), the method of the prior art is used.

[0133] The filtration residues of the dispersions in Example 5a and Comparative Example 5b have been measured as explained in Example 2. The results are shown in Table 7 below. Example 5a Comparative Example 5b Filter residue 2.1% by weight, based on the total weight of the dispersion. 35.9% by weight, based on the total weight of the dispersion. Table 7

[0134] Therefore, Examples 5a and 5b confirm that filter residues can be reduced when using the method of the present invention.

[0135] Furthermore, the β-carotene content of the dispersion in Example 5a was determined by UV / VIS. The content was measured at 7.3% by weight, based on the total weight of the dispersion. If this dispersion is spray-dried, the resulting powder is expected to have a β-carotene content of approximately 24.0% by weight, based on the total weight of the powder. Examples 6a and 6b (gelatin)

[0136] Examples 1a and 1b were repeated. However, this time a different type of emulsifier / colloid (gelatin instead of modified starch) was used. A comparison of the compositions used in Examples 1a / 1b and Examples 6a / 6b is shown in Table 8 below. Example 1a / 1b Example 6a / 6b The composition in container (3) at the start of the method beta-carotene dl-α-tocopherol corn oil Ethyl acetate beta-carotene dl-α-tocopherol corn oil Ethyl acetate The composition in container (4) at the start of the method HiCap® water Fish gelatin (dried) sucrose Ascorbyl palmitate water Table 8

[0137] In Example 6a, the method of the present invention is used. In Example 6b (=Comparative Example), the method of the prior art is used.

[0138] The filtration residues of the dispersions in Example 6a and Comparative Example 6b have been measured as explained in Example 2. The results are shown in Table 9 below. Example 6a Comparison Example 6b Filter residue 1.6% by weight, based on the total weight of the dispersion. 79.9% by weight, based on the total weight of the dispersion. Table 9

[0139] Therefore, Examples 6a and 6b confirm that filter residues can be reduced when using the method of the present invention.

[0140] Furthermore, the β-carotene content of the dispersion of Example 6a was determined by UV / VIS. The content was measured to be 14.9% by weight, based on the total weight of the dispersion. If this dispersion is spray-dried, the resulting powder is expected to have a β-carotene content of approximately 37.1% by weight, based on the total weight of the powder.

[0141] Example 6 clearly demonstrates that the technical effect of the present invention is particularly evident when a highly concentrated powder is to be manufactured.

[0142] From the above discussion, it will be understood that the present invention can be embodied in various forms, including but not limited to the following: Example 1: An arrangement comprising an evaporator (1), a mixing unit (2), a container (3), a container (4) and a mixing unit (5), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b) and a liquid outlet (1c), and wherein the evaporator (1), the mixing unit (2), the container (3) and the mixing unit (5) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2) and from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1), characterized in that the container (4) is configured such that a liquid composition can be fed from the container (4) to the mixing unit (2) and to the mixing unit (5). Example 2: As in Example 1, wherein the arrangement includes components for controlling the flow from container (4) to mixing unit (2) and / or to mixing unit (5), and wherein the arrangement preferably includes a pump for controlling the flow from container (4) to mixing unit (2) and / or wherein the arrangement preferably includes a pump for controlling the flow from container (4) to mixing unit (5), and / or wherein the arrangement includes components for controlling the flow from container (3) to mixing unit (2), and wherein container (3) preferably has a pump for controlling the flow from container (3) to mixing unit (2). Example 3: As in Example 1 or 2, wherein the container (4) is connected to the mixing unit (5) by a connector (4a), wherein the connector (4a) is preferably a pipe, a conduit, a channel, a funnel, a flow path, a conduit, or a groove, and / or wherein the connector (4a) preferably has a length of at least 2 meters, more preferably at least 10 meters, and most preferably at least 100 meters. Example 4: As in any of Examples 1 to 3, wherein each of the containers (3) and (4) is capable of holding a volume of at least 100 liters, more preferably at least 500 liters, and most preferably at least 3000 liters.Example 5: An arrangement comprising an evaporator (1), a mixing unit (2), a container (3), a mixing unit (5), and an evaporator (6), wherein the evaporator (1) has a feed inlet (1a), a steam outlet (1b), and a liquid outlet (1c), and wherein the evaporator (6) has a feed inlet (6a), a steam outlet (6b), and a liquid outlet (6c), and wherein the evaporator (1), mixing unit (2), container (3), mixing unit (5), and evaporator (6) are configured such that a liquid composition can be fed from the container (3) to the mixing unit (2), and fed from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1), and fed from the mixing unit to the evaporator (6) via the feed inlet (6a) of the evaporator (6). The feature is that the configuration is as described in any of Examples 1 to 4, or the configuration further includes a container (4') and a container (4''), wherein the container (4') is configured such that a liquid composition can be fed from the container (4') into the mixing unit (2), and / or wherein the container (4'') is configured such that a liquid composition can be fed from the container (4'') into the mixing unit (5). Example 6: The configuration is as described in Example 5, further including a mixing unit (7), wherein the mixing unit (7) is configured such that a liquid composition can be fed from the evaporator (6) into the mixing unit (7) via a liquid outlet (6c). Example 7: As in Example 6, it further includes an evaporator (8) having a feed inlet (8a), a vapor outlet (8b), and a liquid outlet (8b), wherein the evaporator (8) is configured such that a liquid composition can be fed from the mixing unit (7) into the evaporator (8) via the feed inlet (8a). Example 8: As in any of Examples 1 to 7, wherein the mixing unit (2), mixing unit (5), and / or mixing unit (7) is a homogenizer device, and wherein the homogenizer device is preferably a homogenizer having a pressure drop of at least 50 bar, a colloid mill, a nozzle, a rotor-stator, or a combination thereof. Example 9: As in any of Examples 1 to 8, wherein the evaporator (1), evaporator (6), and / or evaporator (8) is adapted to remove an organic solvent and / or is a vertical evaporator, a thin-film evaporator, or a flash evaporator. Example 10: The setup of any of Examples 1 to 9 further includes an apparatus for spray drying, such as a spray drying tower.Example 11: A method for preparing a powder comprising at least one fat-soluble compound, wherein the method comprises the steps of a) providing a solution comprising at least one fat-soluble compound, at least one solvent, and optionally at least one oil; b) providing a composition comprising water and at least one emulsifier; c) adding a portion of the solution of step a) to a portion of the solution of step b) under vigorous stirring; d) removing at least partially the at least one solvent by heating the composition of step c) at a pressure of less than 1500 mbar; e) adding an additional portion of the composition of step a) to the composition of step d) under vigorous stirring; and f) removing at least partially the at least one solvent by heating the composition of step e) at a pressure of less than 1500 mbar. Example 12: The method of Example 11, further comprising the steps of g) adding an additional portion of the composition of step a) to the composition of step f) under vigorous stirring; and h) removing at least partially the at least one solvent by heating the composition of step g) at a pressure of less than 1500 mbar. Example 13: The method of Example 11 or 12, wherein the setup of any one of Examples 1 to 10 is used, and wherein the solution provided in step a) is placed in a container (4) or container (4') and container (4'') of any one of Examples 1 to 10, and / or wherein the composition provided in step b) is placed in a container (3) of any one of Examples 1 to 10. Example 14: The method of any one of Examples 12 to 13, wherein the solvent is at least one water-immiscible organic solvent, preferably dichloromethane, ethyl acetate or isopropyl acetate, and / or wherein the fat-soluble compound is an edible colorant, preferably β-carotene or lycopene. Example 15: A composition obtained in step f) of the method of any one of Examples 11 to 14 or a composition obtained in step g) of the method of any one of Examples 12 to 14. [Simplified Explanation of the Diagram]

[0018] Figure 1 shows the scheme of the method used in the comparative example. It is a linear method with only one evaporation step. This evaporation step is performed to remove the solvent.

[0019] Figure 2 illustrates a drawback of the method used in the comparative example: attempts to increase the amount of the fat-soluble compound (which also requires a larger amount of solvent to dissolve the fat-soluble compound) failed because the particles collapsed last during the evaporation step. In Figure 2, the particles are shown in the aqueous phase of the liquid composition. The liquid composition is located in an open container. The fat-soluble compound (pentagonal), oil (triangular), and solvent (elliptical) are sealed by a shell (circular; dashed line). The shell contains an emulsifier.

[0020] Figure 3 illustrates the concept of "critical emulsification mass ratio" using a hypothetical system with a critical emulsification mass ratio of 0.55. As the relative amounts of solvent and lipophilic compounds increase, the critical emulsification mass ratio of the system eventually exceeds. If the critical emulsification ratio of the system is exceeded, the filter residue becomes unacceptably high after solvent removal. In the selected hypothetical system, there is no oil, meaning the lipophilic compounds are both solvent and lipophilic compounds. The hydrophilic matrix of the selected hypothetical system consists of water and emulsifiers; that is, the hydrophilic matrix does not contain other optional compounds.

[0021] Figure 4 is a graphical illustration of the general principles of the present invention. It illustrates how filtration residues can be kept low, even if the system has a high content of fat-soluble compounds. Solvent removal is performed in more than one step, i.e., there is more than one evaporation step (compared to Figure 1). Furthermore, an intermediate composition is produced that does not appear in the method shown in Figure 1.

[0022] Figure 5 illustrates why the particles do not collapse when the method of the present invention is used. Compared to the method shown in Figure 2, the formation of core particles and a large amount of solvent is avoided when the emulsification step is broken down into multiple steps separated by the evaporation step.

[0023] Figures 6 to 8 illustrate different embodiments of the configuration of the present invention.

[0024] Figure 6 shows a preferred embodiment of the arrangement of the present invention, which has two evaporators and two mixing units. The evaporator (1) has a feed inlet (1a), a steam outlet (1b) and a liquid outlet (1c). Similarly, the evaporator (6) has a feed inlet (6a), a steam outlet (6b) and a liquid outlet (6c). The liquid outlet (6c) can be connected to equipment for spray drying (not shown in Figure 6). The mixing units (2) and (5) are preferably homogenizers. The mixing unit (2) has an inlet (2a) and an outlet (2b). Similarly, the mixing unit (5) has an inlet (5a) and an outlet (5b). The arrangement shown in Figure 6 further includes a container (3) and a container (4). In the embodiment of Figure 6, the evaporator (1), mixing unit (2), container (3), mixing unit (5), and evaporator (6) are configured such that the liquid composition can be fed from the container (3) into the mixing unit (2) and from the mixing unit (2) into the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) into the mixing unit (5) via the liquid outlet (1c) of the evaporator (1) and from the mixing unit (5) into the evaporator (6) via the feed inlet (6a) of the evaporator (6). The container (4) is configured such that the liquid composition can be fed from the container (4) into both mixing units, i.e., into the mixing unit (2) and the mixing unit (5). The container (4) is connected to the mixing unit (5) by a connector (4a). The connector (4a) may be a pipe, pipe, channel, funnel, flow path, conduit, or trough. The setup shown in Figure 6 includes components for controlling the flow from container (4) to mixing unit (2) and mixing unit (5). These components may be pumps.

[0025] Figure 7 illustrates an even preferred embodiment of the arrangement of the present invention, which has three evaporators and three mixing units. Therefore, the arrangement shown in Figure 7 is an extended version of the arrangement shown in Figure 6. Similar to evaporators (1) and (6), evaporator (8) has a feed inlet (8a), a steam outlet (8b), and a liquid outlet (8c). The mixing unit (7) has an inlet (7a) and an outlet (7b), similar to mixing units (5) and (2). The arrangement shown in Figure 7 includes containers (3) and (4), similar to the embodiment shown in Figure 6. In the embodiment of FIG7, the evaporator (1), mixing unit (2), container (3), mixing unit (5), evaporator (6), mixing unit (7) and evaporator (8) are configured such that the liquid composition can be fed from the container (3) to the mixing unit (2) and from the mixing unit (2) to the evaporator (1) via the feed inlet (1a) of the evaporator (1) and from the evaporator (1) to the mixing unit (5) via the liquid outlet (1c) of the evaporator (1) and from the mixing unit (5) to the evaporator (6) via the feed inlet (6a) of the evaporator (6) and from the evaporator (6) to the mixing unit (7) via the liquid outlet (6c) of the evaporator (6) and from the mixing unit (7) to the evaporator (8) via the feed inlet (8a) of the evaporator (8). The container (4) is configured to allow the liquid composition to be fed from the container (4) into all three mixing units, namely, into mixing unit (2), mixing unit (5), and mixing unit (7). The container (4) is connected to mixing unit (5) via connector (4a) and to mixing unit (7) via connector (4b). Connectors (4a) and (4b) may be pipes, pipes, channels, funnels, flow paths, conduits, or tubing. The arrangement shown in Figure 7 includes a component for controlling the flow from the container (4) to mixing units (2), (5), and (7). This component may be a pump.

[0026] Figure 8 shows a second preferred embodiment of the embodiment shown in Figure 7. It also has three evaporators and three mixing units. However, the embodiment shown in Figure 8 has three separate containers: container (4'), container (4''), and container (4'''), instead of container (4). Container (4') is configured such that the liquid composition can be fed from container (4') into mixing unit (2). Container (4'') is configured such that the liquid composition can be fed from container (4'') into mixing unit (5). Container (4''') is configured such that the liquid composition can be fed from container (4''') into mixing unit (7). Container (4'') is connected to mixing unit (5) by connector (4a) and container (4''') is connected to mixing unit (7) by connector (4b). Connectors (4a) and (4b) may be pipes, pipes, channels, funnels, flow paths, conduits, or tubing. The setup shown in Figure 8 includes components for controlling the flow from container (4') to mixing unit (2), components for controlling the flow from container (4'') to mixing unit (5), and components for controlling the flow from container (4''') to mixing unit (7). These components may be pumps.

[0027] In Figures 7 and 8, the liquid outlet (8c) can be connected to equipment for spray drying (not shown in Figures 7 and 8).

[0028] Figure 9 illustrates the meaning of "bimodal". When performing the method of the present invention, it is inevitable that a composition containing two types of particles will appear: some particles contain many solvent molecules in the core (i.e., mode 1) while other particles contain no solvent molecules or very few solvent molecules in the core (mode 2). The mixing of two different unimodal distributions (i.e., distributions with only one mode) produces a bimodal distribution.

[0029] It should be understood that the diagrams are intended for illustrative purposes only. Those familiar with this technique may find the reality to be more complex.

[0030] Furthermore, it should be understood that the drawings do not limit the scope of the invention. For example, Figures 2 and 5 illustrate a system including oil. However, oil is an optional component (see below). This detail, with necessary modifications, also applies to other features shown in the drawings.

Claims

1. An apparatus for preparing spray-dried powder, comprising an evaporator, a first mixing unit, a first container, a second container, and a second mixing unit, wherein the evaporator has a feed inlet, a vapor outlet, and a liquid outlet, and wherein the evaporator, the first mixing unit, the first container, and the second mixing unit are configured such that a liquid composition can be fed from the first container to the first mixing unit and from the first mixing unit to the evaporator via the feed inlet of the evaporator and from the evaporator to the second mixing unit via the liquid outlet of the evaporator, characterized in that the second container is configured such that the liquid composition can be fed from the second container to the first mixing unit and to the second mixing unit.

2. The setting as requested in claim 1, wherein the setting further includes a component for controlling the flow from the second container to or to the first mixing unit, or wherein the setting includes a component for controlling the flow from the first container to the first mixing unit.

3. As requested in item 1 or 2, wherein the second container is connected to the second mixing unit by a connector, or wherein the connector has a length of at least 2 meters.

4. As configured in request item 1, wherein each of the first container and the second container is capable of holding a volume of at least 100 liters.

5. An apparatus for preparing spray-dried powder, comprising a first evaporator, a first mixing unit, a first container, a second mixing unit, and a second evaporator, wherein the first evaporator has a first feed inlet, a first vapor outlet, and a first liquid outlet, and wherein the second evaporator has a second feed inlet, a second vapor outlet, and a second liquid outlet, and wherein the first evaporator, the first mixing unit, the first container, the second mixing unit, and the second evaporator are configured such that a liquid composition can be fed from the first container to the first mixing unit, fed from the first mixing unit to the first evaporator via the first feed inlet of the first evaporator and fed from the first evaporator to the second mixing unit via the first liquid outlet of the first evaporator, and fed from the second mixing unit to the second evaporator via the second feed inlet of the second evaporator. The feature is that the arrangement further includes a second container and a third container, wherein the second container is configured such that a liquid composition can be fed from the second container into the first mixing unit, and / or wherein the third container is configured such that a liquid composition can be fed from the third container into the second mixing unit.

6. As provided in claim 5, it further includes a third mixing unit, wherein the third mixing unit is configured such that the liquid composition can be fed from the second evaporator to the third mixing unit via the second liquid outlet.

7. As provided in claim 6, it further includes a third evaporator having a third feed inlet, a third steam outlet and a third liquid outlet, wherein the third evaporator is configured such that the liquid composition can be fed from the third mixing unit into the third evaporator via the third feed inlet.

8. As requested in item 6, wherein each of the first mixing unit, the second mixing unit and / or the third mixing unit is a homogenizer device.

9. As requested in item 7, wherein each of the first evaporator, the second evaporator and / or the third evaporator is adapted to remove an organic solvent, or is a vertical evaporator, a thin-film evaporator or a flash evaporator.

10. As provided in claim 6, it further includes an apparatus for spray drying.

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