Solid preparation containing beta-carotene

Abstract

The invention relates to a solid preparation containing beta-carotene with high content and specific stereochemical configuration. In addition, the invention also relates to a method for producing said specific formulations.

Description

[0001] The present invention relates to a solid preparation containing beta-carotene, wherein the beta-carotene exists in a high content of a specific stereochemical form (all E form). In addition, the present invention also relates to a method for preparing the specific preparation.

[0002] β-carotene, i.e., a compound of formula (I)

[0003]

[0004] It is an important and useful compound. The compound of formula (I) is present in the form of "all E" stereochemistry.

[0005] Due to the carbon-carbon double bonds in its structure, β-carotene exists in a variety of stereochemical forms.

[0006] The all-E form (shown above) is highly desirable. This stereochemical form of beta-carotene is considered to be the most bioavailable form.

[0007] In addition, all-E-type β-carotene has better provitamin A activity than other stereochemical forms.

[0008] In the body, beta-carotene is converted into vitamin A (retinol). Vitamin A is essential for good vision and eye health, a strong immune system, and healthy skin and mucous membranes.

[0009] In addition to its health benefits, beta-carotene can also be used as a colorant, especially for coloring foods and beverages.

[0010] β-Carotene itself can be derived from natural sources or produced by chemical or biochemical methods.

[0011] Because beta-carotene has so many applications, it needs to be formulated. This means putting the beta-carotene into a formulation that is suitable for a specific application.

[0012] β-carotene can be formulated into liquid emulsions or solid preparations, such as spray-dried powders, granules, pellets or similar dry product preparations. These preparations can be used directly or further formulated into final product forms.

[0013] The present invention relates to specific solid dosage forms.

[0014] The solid preparation of the present invention can be applied to food, beverage, animal feed product, consumer product or health product.

[0015] To prepare a solid preparation, an emulsion / dispersion containing β-carotene is usually prepared in a first step and then converted into a solid preparation in a second step by commonly known techniques such as drying, spray drying, etc.

[0016] When producing preparations containing β-carotene, a problem arises that β-carotene readily isomerizes into various stereochemical forms.

[0017] The object of the present invention is to provide a solid preparation containing β-carotene, wherein the content of β-carotene in the important all-E configuration is at least 55% (based on the total content of β-carotene).

[0018] Therefore, the present invention relates to a solid dosage form (SF) comprising

[0019] (i) beta-carotene, and

[0020] (ii) at least one hydrogel, and

[0021] (iii) tocopherol, and

[0022] (iv) optional water

[0023] (v) optionally, at least one additional ingredient,

[0024] (vi) optional coating,

[0025] Characterized in that at least 55 weight-% (wt-%) of the β-carotene (based on the total weight of the β-carotene) is in the all-E form.

[0026] The beta-carotene used in the preparation of the present invention may come from any source. This means that the beta-carotene may come from natural sources or may be produced by chemical synthesis or biotechnological methods.

[0027] It is also possible to use nature-identical β-carotene and natural β-carotene mixtures from the above-mentioned production methods.

[0028] The source of the beta-carotene is not critical to the present invention.

[0029] It is essential for the present invention that the content of total E-type β-carotene is at least 55 wt-%, based on the total weight of β-carotene.

[0030] Preferably, the content of total E-type β-carotene is at least 58 wt-%, based on the total weight of β-carotene; more preferably, the content of total E-type β-carotene is at least 60 wt-%, based on the total weight of β-carotene; particularly preferably, the content of total E-type β-carotene is at least 62 wt-%, based on the total weight of β-carotene.

[0031] Preferably, the solid formulation (SF) is obtained by using a spray granulation process, preferably by using a spray granulation step starting from a liquid emulsion comprising at least components (i) to (iii) of the solid formulation and optionally components (iv) and (v).

[0032] Therefore, the present invention relates to a solid preparation (SF1) which is a preparation (SF) wherein the content of total E-type β-carotene is at least 58 wt-%, based on the total weight of β-carotene.

[0033] Therefore, the present invention relates to a solid preparation (SF1') which is a preparation (SF) wherein the content of total E-type β-carotene is at least 60 wt-%, based on the total weight of β-carotene.

[0034] Therefore, the present invention relates to a solid preparation (SF1") which is a preparation (SF) wherein the content of total E-type β-carotene is at least 62 wt-%, based on the total weight of β-carotene.

[0035] The overall content of beta-carotene in the solid preparation of the present invention is 0.5 to 25 wt-% based on the total weight of the solid preparation.

[0036] Preferably, the total content of β-carotene in the solid preparation of the present invention is 1 to 25 wt-%, based on the total weight of the solid preparation.

[0037] More preferably, the total content of β-carotene in the solid preparation of the present invention is 1 to 20 wt-%, based on the total weight of the solid preparation.

[0038] It is particularly preferred that the total content of beta-carotene in the solid preparation of the present invention is 1 to 15 wt-%, based on the total weight of the solid preparation.

[0039] Most preferably, the total content of β-carotene in the solid preparation of the present invention is 2 to 15 wt-%, based on the total weight of the solid preparation.

[0040] Therefore, the present invention relates to a solid preparation (SF2), which is preparation (SF), (SF1), (SF1') or (SF1"), wherein the content of β-carotene in the solid preparation is 0.5 to 25 wt-%, based on the total weight of the solid preparation.

[0041] Therefore, the present invention relates to a solid formulation (SF2'), which is a formulation (SF), (SF1), (SF1') or (SF1"), wherein the content of beta-carotene in the solid formulation is 1 to 25 wt-%, based on the total weight of the solid formulation.

[0042] Therefore, the present invention relates to a solid preparation (SF2"), which is a preparation (SF), (SF1), (SF1') or (SF1"), wherein the content of beta-carotene in the solid preparation is 1 to 20 wt-%, based on the total weight of the solid preparation.

[0043] Therefore, the present invention relates to a solid preparation (SF2'"), which is a preparation (SF), (SF1), (SF1') or (SF1"), wherein the content of beta-carotene in the solid preparation is 1 to 15 wt-%, based on the total weight of the solid preparation.

[0044] Therefore, the present invention relates to a solid preparation (SF2″"), which is preparation (SF), (SF1), (SF1'), (SF1") or (SF1'"), wherein the content of β-carotene in the solid preparation is 2 to 15 wt-%, based on the total weight of the solid preparation.

[0045] The solid preparation of the present invention comprises at least one hydrogel. The hydrogel in the present invention has emulsifying properties.

[0046] In the context of the present invention, hydrogels refer to polysaccharides, low, medium or high Bloom value gelatin from fish, pork or beef, casein / caseinates, plant or animal based proteins, other protein hydrogels and lignin sulfonates.

[0047] According to the present invention, preferred hydrogels are polysaccharides.

[0048] In the context of the present invention, the term "polysaccharide" as used herein includes xanthan gum, gum arabic, pectin, guar gum, carob gum, algin, cellulose, cellulose derivatives (such as starch and starch derivatives). Preferred polysaccharides of the present invention are gum arabic, starch, starch derivatives, more preferably gelatinized starch and modified edible starch, and particularly preferably modified edible starch.

[0049] In the context of the present invention, the term "modified edible starch" as used herein refers to a modified starch prepared by replacing starch with a hydrophobic group by a known chemical method. For example, starch can be treated with a cyclic dicarboxylic acid anhydride (such as succinic anhydride and / or glutaric anhydride) and replaced with an alkyl or olefin group.

[0050] A very common and preferred modified starch is sodium starch octenyl succinate (OSA-starch). As used herein, OSA-starch refers to any starch (from any natural source, such as corn, wheat, cassava, potato or synthetic source) treated with octenyl succinic anhydride. The degree of substitution, i.e. the ratio of the number of esterified hydroxyl groups to the total number of hydroxyl groups, generally varies in the range of 0.1% to 10%, preferably in the range of 0.5% to 5%, more preferably in the range of 2% to 4%.

[0051] OSA-starch is commercially available, for example, from Ingredion under the trade names HiCap 100, Capsul HF, Capsul HS, Purity Gum 2000, UNI-PURE, HYLON VII; from Roquette Freres; from Cargill under the trade name C*EmCap; or from Tate & Lyle.

[0052] The at least one hydrogel is generally present in an amount of 40 to 90 wt-%, preferably 45 to 90 wt-%, more preferably 50 to 90 wt-%, based on the total weight of the solid formulation.

[0053] Therefore, the present invention relates to a solid formulation (SF3), which is a solid formulation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"') or (SF2""), wherein the at least one hydrogel is selected from the group consisting of polysaccharides, gelatin with low, medium or high Bloom value from fish, pork or beef, casein / caseinate, plant or animal based proteins, other protein hydrogels and lignin sulfonates.

[0054] Therefore, the present invention relates to a solid formulation (SF3') which is a solid formulation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"') or (SF2""), wherein the at least one hydrogel is selected from the group consisting of xanthan gum, gum arabic, pectin, guar gum, carob gum, alginate, cellulose, cellulose derivatives such as starch and starch derivatives.

[0055] Therefore, the present invention relates to a solid preparation (SF3"), which is a solid preparation (SF), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"') or (SF2""), wherein the hydrogel is modified edible starch.

[0056] Therefore, the present invention relates to a solid preparation (SF3'"), which is a solid preparation (SF3"), wherein the modified edible starch is sodium starch octenylsuccinate.

[0057] Therefore, the present invention relates to a solid formulation (SF4), which is a solid formulation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3") or (SF3"'), wherein the content of the at least one hydrogel is 40 to 90 wt-%, based on the total weight of the solid formulation.

[0058] Therefore, the present invention relates to a solid formulation (SF4'), which is a solid formulation (SF), (SF1), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3") or (SF3"'), wherein the content of the at least one hydrogel is 45 to 90 wt-%, based on the total weight of the solid formulation.

[0059] Therefore, the present invention relates to a solid formulation (SF4"), which is a solid formulation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3") or (SF3"'), wherein the content of the at least one hydrogel is 50 to 90 wt-%, based on the total weight of the solid formulation.

[0060] The solid preparation of the present invention contains tocopherol.

[0061] In the context of the present invention, the term "tocopherol" encompasses any of its eight stereoisomers, ie, all-rac-α-tocopherol, including D / L-α-tocopherol and mixed tocopherols.

[0062] Based on the total weight of the solid preparation, the content of tocopherol is 0.1 to 5 wt-%, preferably 0.1 to 4 wt-%, more preferably 0.5 to 3 wt-% of the total weight of the solid preparation.

[0063] Therefore, the present invention relates to a solid preparation (SF5), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4') or (SF4'), wherein the tocopherol content is 0.1 to 5 wt-% of the total weight of the solid preparation.

[0064] Therefore, the present invention relates to a solid preparation (SF5'), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4') or (SF4'), wherein the tocopherol content is 0.1 to 4 wt-% of the total weight of the solid preparation.

[0065] Therefore, the present invention relates to a solid preparation (SF5"), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4') or (SF4'), wherein the tocopherol content is 0.5 to 3 wt-% based on the total weight of the solid preparation.

[0066] The solid preparation of the present invention may contain a certain amount of water (residual water). The content of residual water may vary depending on the type and characteristics of the drying method used to dry the solid preparation.

[0067] The moisture content of the solid preparation of the present invention is less than 8 wt-% of the total weight of the solid preparation.

[0068] Preferably, the water content of the solid preparation of the present invention is less than 7 wt-%, more preferably less than 6 wt-%, particularly preferably less than 5 wt-%, based on the total weight of the solid preparation.

[0069] Therefore, the present invention relates to a solid formulation (SF6), which is a solid formulation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5') or (SF5"), wherein the water content is less than 8 wt-%, based on the total weight of the solid formulation.

[0070] Therefore, the present invention relates to a solid formulation (SF6'), which is a solid formulation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5') or (SF5"), wherein the water content is less than 7 wt-%, based on the total weight of the solid formulation.

[0071] Therefore, the present invention relates to a solid preparation (SF6"), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"), (SF2"), (SF2"), (SF3), (SF3'), (SF3"), (SF3"), (SF4), (SF4'), (SF4'), (SF5), (SF5') or (SF5"), wherein the water content is less than 6 wt-%, based on the total weight of the solid preparation.

[0072] Therefore, the present invention relates to a solid preparation (SF6"'), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5') or (SF5"), wherein the water content is less than 5 wt-%, based on the total weight of the solid preparation.

[0073] The solid preparation of the present invention may optionally include at least one other component. These components may be starch hydrolysate (such as dextrin, maltodextrin and glucose syrup), oil (such as coconut oil, sunflower oil, corn oil, medium chain triglyceride oil (MCT oil) and other vegetable oils), dye, filler, adhesive, flavoring agent, etc.

[0074] These additional ingredients may be present in an amount of up to 15% (wt-%) based on the total weight of the solid preparation.

[0075] Therefore, the present invention relates to a solid preparation (SF7), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6") or (SF6"'), wherein the solid preparation comprises at least one additional ingredient selected from starch hydrolysate (such as dextrin, maltodextrin and glucose syrup), oil (such as coconut oil, sunflower oil, corn oil, medium chain triglyceride (MCT) oil and other vegetable oils), dyes, fillers, adhesives and fragrances.

[0076] Therefore, the present invention relates to a solid preparation (SF8), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"') or (SF7), wherein the content of the at least one additional ingredient does not exceed 15 wt-%, based on the total weight of the solid preparation.

[0077] The solid preparation of the present invention may be subjected to coating treatment, that is, the surface thereof may have a coating.

[0078] The coating can be any common coating. It can be a powder coating. Such a powder coating can be made of starch (such as corn starch).

[0079] The coating may comprise up to 45% (wt-%) of the solid formulation, based on the total weight of the solid formulation.

[0080] Therefore, the present invention relates to a solid preparation (SF9), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7) or (SF8), wherein the solid preparation is coated with a coating.

[0081] Therefore, the present invention relates to a solid preparation (SF9'), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7) or (SF8), wherein the solid preparation is coated with a powder coating.

[0082] Therefore, the present invention relates to a solid preparation (SF10), which is a solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7), (SF8), (SF9) or (SF9'), wherein, based on the total weight of the solid preparation, the maximum proportion of the coating to the weight of the solid preparation is 45%.

[0083] Obviously, for one embodiment of the present invention, the sum of the various values ​​always amounts to 100%.

[0084] The solid preparation according to the present invention may be in the form of powder, granules or microbeads.

[0085] The particle size of the solid preparation may be between 50 microns and 1000 microns.

[0086] The particle size distribution of the powder preparation can be measured based on the average Sutter diameter D(3;2) using a laser diffractometer Mastersizer 3000 (Malvern Instruments, Malvern, United Kingdom) using the Fraunhofer model.

[0087] Particle size can vary, depending on a variety of factors such as production method, intended use, etc.

[0088] The solid preparations (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7), (SF8), (SF9), (SF9') or (SF10) according to the present invention can be used directly or further formulated into the final product.

[0089] The solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7), (SF8), (SF9), (SF9') or (SF10) according to the present invention can be used in food, feed products, dietary supplements, medicines and / or personal care products.

[0090] Furthermore, the present invention relates to food, feed products, dietary supplements, pharmaceuticals and personal care products comprising at least one solid dosage form (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7), (SF8), (SF9), (SF9') or (SF10).

[0091] The solid preparation according to the present invention can be produced by a known method.

[0092] Generally, the production steps of the solid preparation (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7), (SF8), (SF9), (SF9') or (SF10) according to the present invention are as follows:

[0093] Step (i): emulsifying / dispersing / dissolving β-carotene, and

[0094] Step (ii): Producing a solid form from the emulsion / dispersion of step (i).

[0095] Therefore, the present invention relates to a method (P) for producing a solid dosage form (SF), (SF1), (SF1'), (SF1"), (SF2), (SF2'), (SF2"), (SF2"'), (SF2""), (SF3), (SF3'), (SF3"), (SF3"'), (SF4), (SF4'), (SF4'), (SF5), (SF5'), (SF5"), (SF6), (SF6'), (SF6"), (SF6"'), (SF7), (SF8), (SF9), (SF9') or (SF10), comprising

[0096] Step (i): emulsifying / dispersing / dissolving β-carotene, and

[0097] Step (ii): Producing a solid form from the emulsion / dispersion of step (i).

[0098] These steps are discussed in more detail below.

[0099] Step (i)

[0100] The beta-carotene is dissolved in a solvent and / or a solvent mixture.

[0101] Suitable solvents are organic solvents, preferably organic solvents having a boiling point below 150° C., more preferably below 140° C., in particular below 120° C. at 1013.25 hPa.

[0102] A preferred solvent is isobutyl acetate.

[0103] In the context of the present invention, a "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 typical embodiments of the present invention, the core of the particles of the dispersion comprises both liquid and solid compounds.

[0104] The "particles" of the dispersion are too small to be seen with the naked eye. In a preferred embodiment of the invention, the average particle size of the particles is in the range of 50 to 1000 nanometers, more preferably 100 to 800 nanometers, further preferably 100 to 500 nanometers [average particle diameter measured by dynamic light scattering (Beckman Coulter, Delsa Nano S)]. Despite having a lipophilic core, the particles are still dispersible in water. This is achieved by surrounding the core with at least one hydrophilic colloid having emulsifying properties (component (ii)). This surrounding is called the shell of the particle.

[0105] An aqueous solution is also prepared, comprising water and at least one hydrophilic colloid (component (ii)).

[0106] Obviously, all the preferences for hydrocolloids stated previously apply here as well.

[0107] Preferably, the at least one hydrocolloid is selected from xanthan gum, gum arabic, pectin, guar gum, carob gum, alginate, cellulose, cellulose derivatives such as starch and starch derivatives.

[0108] More preferably, the hydrocolloid is modified edible starch.

[0109] Most preferably, the hydrocolloid is sodium starch octenylsuccinate.

[0110] Finally, the two phases are mixed, usually under vigorous stirring and / or high pressure homogenization conditions, to obtain a dispersion / emulsion.

[0111] Obviously, the β-carotene phase and the aqueous phase may also contain other (optional) ingredients, such as starch hydrolysates (such as dextrins, maltodextrins and glucose syrups), oils (such as coconut oil, sunflower oil, corn oil, medium chain triglyceride oils and other vegetable oils), dyes, fillers, binders and fragrances.

[0112] According to step (ii), the viscosity of the dispersion / emulsion needs to be within a certain range in order to carry out the granulation step.

[0113] The present invention therefore relates to a process (P1) which is process (P), wherein the beta-carotene is dissolved in at least one solvent having a boiling point below 150°C.

[0114] The present invention therefore relates to a process (P1') which is process (P), wherein the beta-carotene is dissolved in at least one solvent having a boiling point below 140°C.

[0115] The present invention therefore relates to a process (P1") which is process (P), wherein the beta-carotene is dissolved in at least one solvent having a boiling point below 120°C.

[0116] The present invention therefore relates to a process (P1''") which is process (P), wherein β-carotene is dissolved in isobutyl acetate.

[0117] Therefore, the present invention relates to a process (P2) which is process (P), (P1), (P1'), (P1") or (P1'"), wherein an aqueous solution is prepared comprising water and at least one hydrophilic colloid.

[0118] Therefore, the present invention relates to a method (P2') which is method (P), (P1), (P1'), (P1") or (P1'"), wherein the prepared aqueous solution comprises water and at least one hydrophilic colloid, and the at least one hydrophilic colloid is selected from the group consisting of xanthan gum, gum arabic, pectin, guar gum, carob gum, alginate, cellulose, cellulose derivatives (such as starch and starch derivatives).

[0119] Therefore, the present invention relates to a method (P2") which is method (P), (P1), (P1'), (P1") or (P1'"), wherein the prepared aqueous solution comprises water and at least one hydrocolloid, and the at least one hydrocolloid is a modified food starch.

[0120] Therefore, the present invention relates to a method (P2'") which is method (P), (P1), (P1'), (P1") or (P1'"), wherein the prepared aqueous solution comprises water and at least one hydrophilic colloid, and the at least one hydrophilic colloid is sodium starch glycolate.

[0121] Step (ii)

[0122] In step (ii), a solid form is formed from the emulsion / dispersion of step (i). This is accomplished by a granulation process, more preferably a spray granulation process.

[0123] Granulation is a process of layering small particles with a liquid containing solids to create larger powder particles.

[0124] The granulation process is carried out by spraying the emulsion onto seed particles (produced by emulsion spray drying) for at least 30 minutes (up to several hours), followed by a drying stage of at least 30 minutes (up to 2 hours) at a product temperature of 70°C to 100°C (preferably 75°C to 90°C, most preferably about 80°C).

[0125] Liquid emulsions are granulated by spraying in two steps:

[0126] i) preparing the seed material using spray drying with an inlet air temperature of 160°C to 190°C and an outlet air temperature of 70°C to 100°C (preferably 75°C to 90°C, most preferably about 80°C),

[0127] ii) The granules are prepared using a fluidized bed processor, for example a fluidized bed processor of the WFP-Mini type (DMR Prozess-Technologie GmbH).

[0128] Therefore, the present invention relates to a process (P3) which is process (P), (P1), (P1'), (P1"), (P2), (P2'), (P2") or (P2'"), wherein the liquid emulsion is spray granulated in two steps:

[0129] i) preparing the seed material using spray drying, with an inlet air temperature of 160°C to 190°C and an outlet air temperature of 70°C to 100°C,

[0130] ii) Preparation of granules using a fluidized bed processor.

[0131] Therefore, the present invention relates to a process (P3') which is process (P), (P1), (P1'), (P1"), (P2), (P2'), (P2") or (P2'"), wherein the liquid emulsion is spray granulated in two steps:

[0132] i) preparing the seed material using spray drying, with an inlet air temperature of 160°C to 190°C and an outlet air temperature of 75°C to 90°C,

[0133] ii) Preparation of granules using a fluidized bed processor.

[0134] The present invention therefore relates to a process (P3") which is process (P), (P1), (P1'), (P1"), (P2), (P2'), (P2") or (P2'"), wherein the liquid emulsion is spray granulated in two steps:

[0135] i) preparing the seed material using spray drying with an inlet air temperature of 160°C to 190°C and an outlet air temperature of about 80°C,

[0136] ii) Preparation of granules using a fluidized bed processor.

[0137] Therefore, the present invention relates to a process (P4) which is process (P), (P1), (P1'), (P1"), (P2), (P2'), (P2"), (P2"'), (P3), (P3') or (P3"), wherein the granulation process is carried out for at least 30 minutes (at most several hours) and is followed by a drying phase of at least 30 minutes (at most 2 hours) at a product temperature of 70°C to 100°C.

[0138] Therefore, the present invention relates to a process (P4') which is process (P), (P1), (P1'), (P1"), (P2), (P2'), (P2"), (P2"'), (P3), (P3') or (P3"), wherein the granulation process is carried out for at least 30 minutes (at most several hours) and is followed by a drying phase of at least 30 minutes (at most 2 hours) at a product temperature of 75°C to 90°C.

[0139] Therefore, the present invention relates to a process (P4") which is process (P), (P1), (P1'), (P1"), (P2), (P2'), (P2"), (P2"'), (P3), (P3') or (P3"), wherein the granulation process is carried out for at least 30 minutes (at most several hours) and is followed by a drying phase of at least 30 minutes (at most 2 hours) at a product temperature of about 80°C.

[0140] The following examples further illustrate the present invention without limiting its scope. All percentages and parts given are by weight and temperatures are expressed in ° C. unless otherwise stated. Example

[0141] Embodiment 1:

[0142] 16.5 g of β-carotene and 1.65 g of D / L-α-tocopherol were suspended in 210 ml of isobutyl acetate using a 500 ml three-necked round bottom flask and heated to 115°C for 90 minutes to prepare a solution. For the matrix phase containing the emulsifier, 120 g of OSA modified edible starch was dissolved in 260 ml of water at room temperature in a 1 liter beaker and stirred for 1 hour using conventional vertical stirring. The solution was added to the matrix phase and emulsified at 50-60°C using an IKA G45M rotor stator and an IKAT50 high-speed stirrer at 10,000 rpm for up to 9 minutes.

[0143] The emulsion was transferred to a 2-liter three-necked round-bottom flask and 125 ml of water was added before vacuum evaporation at 40° C. to remove the organic solvent. Vacuum evaporation and eventual further addition of water were continued until the viscosity and residual moisture of the final emulsion reached appropriate levels for the subsequent drying method.

[0144] The emulsion was spray granulated in two steps: i) the seed material was prepared using spray drying in a GEA Niro spray tower (Mobile Minor 2000 Model D1-Spezial) with an inlet air temperature of 180°C and an outlet air temperature of 80°C; ii) the granules were prepared using a WFP-Mini fluidized bed processor (DMR Prozess-Technologie GmbH). The granulation process lasted 3 hours by spraying the emulsion onto the seed granules, followed by drying for 2 hours at a product temperature of 80°C. The spray granulation method increased the (all-E)-isomer ratio from 50-52% of the liquid emulsion to 70% of the final granule product.

[0145] Embodiment 2:

[0146] 33 g of β-carotene and 3.3 g of D / L-α-tocopherol were suspended in 420 ml of isobutyl acetate using a 1 liter three-necked round bottom flask and heated to 115°C for 90 minutes to prepare a solution. For the matrix phase containing the emulsifier, 240 g of OSA modified edible starch was dissolved in 520 ml of water at room temperature in a 2 liter beaker and stirred for 1 hour using conventional vertical stirring. The solution was added to the matrix phase and emulsified at 50-60°C using an IKA G45M rotor stator and an IKA T50 high-speed stirrer at 10,000 rpm for up to 18 minutes.

[0147] The emulsion was transferred to a 4-liter three-necked round-bottom flask and after adding 250 ml of water, the organic solvent was evaporated under vacuum at 40°C. Vacuum evaporation and eventual further addition of water were continued until the viscosity and residual moisture of the final emulsion reached appropriate levels for the subsequent drying method.

[0148] The emulsion was spray granulated in two steps: i) the seed material was prepared using spray drying in a GEA Niro spray tower (Mobile Minor 2000 Model D1-Spezial) with an inlet air temperature of 180°C and an outlet air temperature of 80°C; ii) the granules were prepared using a WFP-Mini fluidized bed processor (DMR Prozess-Technologie GmbH). The granulation process lasted 3 hours by spraying the emulsion onto the seed granules, followed by drying at a product temperature of 80°C for a maximum of 2 hours. The spray granulation method increased the (all-E)-isomer ratio from 50-52% of the liquid emulsion to 70% of the final granule product.

[0149] Embodiment 3:

[0150] The liquid emulsion was prepared according to the work flow described in Examples 1 and 2. The emulsion was spray granulated in two steps: i) the seed material was prepared using spray drying in a GEA Niro spray tower (Mobile Minor 2000 Model D1-Spezial) with an inlet air temperature of 180°C and an outlet air temperature of 80°C; ii) the granules were prepared using a fluidized bed processor of the WFP-Mini type (DMR Prozess-Technologie GmbH). The granulation process lasted for 1.5 hours by spraying the emulsion onto the seed particles, followed by drying at a product temperature of 80°C for 1 hour. The spray granulation process increased the (all-E)-isomer proportion from 52-55% of the liquid emulsion to 63-64% of the final granule product.

[0151] Embodiment 4:

[0152] The liquid emulsion was prepared according to the work flow described in Examples 1 and 2. The emulsion was spray granulated in two steps: i) the seed material was prepared using spray drying in a GEA Niro spray tower (Mobile Minor 2000 Model D1-Spezial) with an inlet air temperature of 180°C and an outlet air temperature of 80°C; ii) the granules were prepared using a WFP-Mini fluidized bed processor (DMR Prozess-Technologie GmbH). The granulation process lasted 1.5 hours by spraying the emulsion onto the seed particles, followed by drying at a product temperature of 80°C for 2 hours. The spray granulation process increased the (all-E)-isomer ratio from 52-55% in the liquid emulsion to 64% in the final granule product.

[0153] Embodiment 5 (comparative example):

[0154] The liquid emulsion was prepared according to the work flow described in Examples 1 and 2. However, in this comparative example, the liquid emulsion was not spray granulated but only spray dried in a GEA Niro spray tower (Mobile Minor 2000 Model D1-Spezial) with an inlet temperature of 180°C and an outlet temperature of 80°C.

[0155] The spray drying process increased the (all-E)-isomer proportion from 52% in the liquid emulsion only to 53% in the spray dried product.

[0156] Comparative Example 6 (Comparative Example):

[0157] The liquid emulsion was prepared according to the work flow described in Examples 1 and 2. However, in this comparative example, the liquid emulsion was not spray granulated but only spray dried in a GEA Niro spray tower (Mobile Minor 2000 Model D1-Spezial) with an inlet temperature of 180°C and an outlet temperature of 80°C.

[0158] The spray drying process increased the (all-E)-isomer proportion from 52% in the liquid emulsion only to 54% in the spray dried product.

[0159] Table 1

[0160] Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 OSA modified edible starch 82.5 82.5 82.5 82.5 82.5 82.5 Beta-carotene 11.3 11.3 11.3 11.3 11.3 11.3 D / L-α-Tocopherol 1.1 1.1 1.1 1.1 1.1 1.1 residual moisture 5.1 5.1 5.1 5.1 5.1 5.1

Claims

1. A method for producing a solid preparation, the solid preparation comprising (i) beta-carotene, and (ii) at least one hydrogel, and (iii) antioxidants, and (iv) optionally, at least one additional ingredient, (v) optional coating, It is characterized in that at least 55% by weight (wt-%) of the beta-carotene (based on the total weight of the beta-carotene) is of the all-E type, Among them, the spray granulation of liquid emulsion is divided into two steps: i) preparing the seed material using spray drying, wherein the air inlet temperature is between 160 and 190°C and the air outlet temperature is between 70 and 100°C, and ii) Preparation of granules using a fluidized bed processor.

2. The method according to claim 1, wherein: The granulation process is carried out for at least 30 minutes (maximum several hours) and is followed by a drying phase at a product temperature of 70°C to 100°C for at least 30 minutes (maximum 2 hours).

3. A solid preparation comprising (i) beta-carotene, and (ii) at least one hydrogel, and (iii) antioxidants, and (iv) optionally, at least one additional ingredient, (v) optional coating, It is characterized in that At least 55 weight-% (wt-%) of the beta-carotene (based on the total weight of the beta-carotene) is of the all-E type, and The solid preparation is obtained by spray granulating a liquid emulsion containing at least the components (i) to (iii) of the solid preparation.

4. The solid preparation according to claim 3, wherein The content of total E-type beta-carotene is at least 58 wt-%, based on the total weight of beta-carotene.

5. The solid preparation according to claim 3, wherein The content of all-E-type beta-carotene is at least 60 wt-%, based on the total weight of beta-carotene.

6. The solid preparation according to any one of the preceding claims 3 to 5, wherein The content of beta-carotene in the solid preparation is 0.5 to 25 wt-%, based on the total weight of the solid preparation.

7. A solid preparation according to any one of claims 3 to 5, wherein The content of beta-carotene in the solid preparation is 1 to 25 wt-%, based on the total weight of the solid preparation.

8. A solid formulation according to any one of the preceding claims 3 to 6, wherein the at least one hydrogel is selected from the group consisting of polysaccharides, low, medium or high Bloom value gelatin from fish, pork or beef, casein / caseinates, plant or animal based proteins, other protein hydrogels and lignin sulfonates.

9. The solid formulation according to any one of the preceding claims 3 to 7, wherein the at least one hydrogel is selected from the group consisting of xanthan gum, gum arabic, pectin, guar gum, carob gum, alginate, cellulose, cellulose derivatives such as starch and starch derivatives.

10. The solid formulation according to any one of the preceding claims 3 to 7, wherein the hydrogel is a modified edible starch.

11. A solid preparation according to any one of claims 3 to 10, wherein The at least one hydrogel is present in an amount of 40 to 90 wt-%, based on the total weight of the solid formulation.

12. A solid preparation according to any one of claims 3 to 11, wherein The antioxidant is tocopherol, and the content of the tocopherol is 0.1 to 5 wt-% based on the total weight of the solid preparation.

13. A solid preparation obtained according to the method of any one of claims 1 or 2.

14. A food, beverage, animal feed product, consumer product or health product comprising the formulation according to any one of claims 3 to 13.

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