CN111493323A - Preparation method of fat-soluble vitamin particles for beverage - Google Patents
Preparation method of fat-soluble vitamin particles for beverage Download PDFInfo
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- CN111493323A CN111493323A CN202010299430.3A CN202010299430A CN111493323A CN 111493323 A CN111493323 A CN 111493323A CN 202010299430 A CN202010299430 A CN 202010299430A CN 111493323 A CN111493323 A CN 111493323A
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Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/15—Vitamins
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/385—Concentrates of non-alcoholic beverages
- A23L2/39—Dry compositions
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/60—Sweeteners
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Mycology (AREA)
- Non-Alcoholic Beverages (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a preparation method of fat-soluble vitamin particles for beverages, which belongs to the field of food additive manufacturing, adopts rubusoside as an auxiliary agent, and prepares vitamin D, vitamin E or mixed particles of the vitamin D and the vitamin E by a solvent method6Multiple and 5-1200 times. The auxiliary agent rubusoside is a safe food additive with the effect of reducing blood sugar, and the method provided by the invention can be used for preparing vitamin D and vitamin E additives in functional foods and beverages.
Description
Technical Field
The invention relates to a preparation method of fat-soluble vitamin particles for beverages, in particular to a process for preparing fat-soluble vitamin particles by using rubusoside as an auxiliary agent and fat-soluble vitamin as a dispersoid, belonging to the field of food additives.
Background
Vitamin E (VE) and Vitamin D (VD) are fat-soluble vitamins. VD has the functions of promoting the absorption of calcium and phosphorus, promoting the mineralization of bones and maintaining the dynamic balance of calcium and phosphorus in blood. In addition, vitamin D also has effects of promoting skin cellularization and regulating immunity. VE has antioxidant ability to scavenge free radicals generated during autoxidation of fats and fatty acids, to protect cell membranes from oxidative damage, and to promote humoral immunity, cellular immunity and phagocytosis by inhibiting the in vivo production of prostaglandins and corticosterones, thereby improving the immunity of the body.
However, both vitamins have poor solubility in water, are insoluble compounds (VD has a solubility of 0.433 μ g/m L and a solubility of 0.007 μ g/m L, data from DRUG BANK), cannot be added to beverages, are not easily dispersed when used for preserving the surface of meat, and are often required to be dissolved in high-concentration ethanol and then sprayed.
Vitamin E is liquid at normal temperature, the nutritional supplement is usually prepared into capsules, and most of the commercially available vitamin D supplements are solid or semisolid preparations. For example, patent CN201711212094.9 discloses a method for preparing vitamin E soft capsules, which comprises preparing stable vitamin E gelatin solution by adding glycerol and gelatin, and then producing vitamin E capsule supplement by the steps of pelleting, shaping, drying, washing, packaging, etc. Patent CN201810127492.9 discloses a method for preparing a capsule containing vitamin E, which comprises sieving vitamin E and medical adjuvants such as hydroxypropyl cellulose and crospovidone, mixing in a mixer, adding appropriate amount of binder to obtain soft material, granulating, drying, and grading. Patent CN201910119036.4 also discloses a method for preparing vitamin D soft capsules. Patent CN201610129310.2 discloses a method for preparing a semisolid preparation containing vitamin D or its derivatives, wherein the mass of vitamin D can only reach 1-5ppm of the mass of the matrix.
The Jinwen yebin (Jinwen yebin, 2017) adopts a series of carboxylic acid ionic liquids (L CC-I L s) with different alkyl chain lengths to solubilize the vitamin E, and 15 percent of L CC-I L s can increase the solubility of the vitamin E to 0.096g/m L at 40 ℃, but the ionic liquid has poor edibility, is unstable in a food system, particularly an electrolyte-containing system, and is used in too large amount, and the Ganyujiang (Ganyujiang, 2013) adopts β -cyclodextrin and derivatives thereof to embed the vitamin D, so that the solubility of the vitamin D can be improved by 4.97 times.
Therefore, the conventional solubilization of vitamin D and vitamin E in water phase still has the disadvantages of difficult operation, poor solubilization effect, difficult practical application and the like. Therefore, a method with simple operation, high safety and good water phase solubilization effect is needed, so as to widen the application range of vitamin D and vitamin E.
Rubusoside (Ru) is a main sweet component in special rare plant sweet tea in Guangxi of China, is a low-energy sweetener, and has sweetness which is 180 times that of cane sugar (150 times of that of cane sugar). The rubusoside is a safe natural sweetener with effects of lowering blood pressure, lowering blood sugar, resisting allergy, inhibiting dental caries, etc.
Disclosure of Invention
[ problem ] to
The technical problems to be solved by the invention are that the solubility of fat-soluble vitamins in water is low, and the application is difficult, such as the application to aqueous beverages is difficult; also, a method for solving the problem of low solubility of fat-soluble vitamins in water is required to be food safe.
[ solution ]
The invention provides a method for greatly improving the solubility of fat-soluble vitamins in water by using a sweetening agent, wherein the sweetening agent is rubusoside.
The present invention also provides a process for preparing fat-soluble vitamin particles useful in beverages comprising the steps of:
(1) dissolving rubusoside in solvent A at a temperature below 10 deg.C below the boiling point of solvent A, and stirring for 30-40min to obtain clear and transparent solution A; dispersing fat-soluble vitamins in solvent B by a homogenizer at a temperature from room temperature to below 15 ℃ lower than the boiling point of the solvent B, and stirring for 30-40min to obtain uniformly dispersed suspension B;
(2) slowly adding the suspension B into the solution A under stirring at 30-60 ℃, mixing to obtain a solution C, continuously stirring the solution C until the solution is completely clear and transparent or is in a uniform and weak light blue white color, further continuously stirring at the same temperature for 30-40min, and then gradually cooling to room temperature under the stirring condition;
(3) and (3) drying the solution C obtained in the step (2) to obtain a white solid, and grinding and sieving the white solid to obtain powder, namely the fat-soluble vitamin granules which can be used in the beverage.
The solvent A is water, ethanol or ethanol water solution, and the solvent B is water, ethanol or ethanol water solution.
The fat-soluble vitamin is one or a mixture of two of vitamin D and vitamin E.
The purity of the rubusoside expressed by HP L C is 60% or more, and the higher the purity of the rubusoside, the larger the usage amount, the better the solubilizing effect of fat-soluble vitamin in water or alcohol-water system.
The mass concentration of the rubusoside in the solution C is not less than 0.4%. The rubusoside may be of plant origin or enzymatically synthesized. For example: rubusoside extracted from commercially available sweet tea, or obtained by enzymatic hydrolysis of steviosides.
The mass concentration of the vitamin E in the solution C is not more than 1 × 10 of the solubility of the vitamin E in a solvent of the solution C (the solvent of the solution C refers to a mixed solvent of the solvent A and the solvent B in the solution C)5The mass concentration of vitamin D is not more than 1000 times its solubility in the solvent of solution C (the solvent of solution C means a mixed solvent of solvent a and solvent B in solution C).
The drying includes freeze drying and vacuum drying. The temperature during vacuum drying does not exceed 35 ℃.
In one embodiment of the present invention, vitamin E is taken as an example, and the following steps are taken:
(1) preparation of rubusoside solution
Dissolving 0.5-2 g of 60% -95% (HP L C purity) rubusoside in water of 15-80m L at 20-90 deg.C, stirring at corresponding dissolving temperature, and dissolving to obtain X m L volume of clear and transparent rubusoside solution;
(2) preparation of vitamin E Dispersion
Dispersing 40-450mg VE in (100-X) m L ethanol water solution at 50 deg.C with a homogenizer, and stirring at dispersing temperature (50 deg.C) to obtain uniformly dispersed vitamin E suspension;
(3) mixing rubusoside solution and vitamin E dispersion
Slowly adding the vitamin E suspension into the rubusoside solution under stirring at 40-50 deg.C, stirring to obtain rubusoside-vitamin E solution, stirring until the solution is clear and transparent, and stirring for 30-40 min; the obtained rubusoside-VE solution is subjected to rotary evaporation under reduced pressure and then freeze drying to obtain white solid, and the white solid is ground and sieved by a 200-mesh sieve to obtain powder, namely the vitamin E particles which can be used in beverages.
In one embodiment of the present invention, taking vitamin D as an example, the following steps are taken:
(1) preparation of rubusoside solution
Dissolving 0.5-2 g of 60% -95% (HP L C purity) rubusoside in water of 15-30m L at 20-90 deg.C, stirring at corresponding dissolving temperature, and dissolving to obtain X m L volume of clear and transparent rubusoside solution;
(2) preparation of vitamin D Dispersion
Dispersing 3-8mg VD in (100-X) m L ethanol water solution by a homogenizer at 50 ℃, and stirring at the dispersion temperature (50 ℃) to obtain uniformly dispersed vitamin D suspension;
(3) mixing rubusoside solution and vitamin D dispersion
Slowly adding the vitamin D suspension into the rubusoside solution under stirring at 40-50 deg.C, stirring to obtain rubusoside-vitamin D solution, stirring until the solution is clear and transparent, and stirring for 30-40 min; and (3) carrying out reduced pressure rotary evaporation on the obtained rubusoside-VD solution, then carrying out vacuum drying to obtain a white solid, grinding the white solid and sieving the white solid with a 200-mesh sieve to obtain powder, namely the vitamin D particles used in the beverage.
The invention also provides application of the VD and VE particles taking rubusoside as a carrier as VD and VE additives in functional food and/or beverage.
[ advantageous effects ]
The conventional method for solubilizing the fat-soluble vitamin in water or an alcohol-water system in the prior art has the defects of difficult operation, poor solubilizing effect, difficult practical application and the like. The method realizes the solubilization of fat-soluble vitamins in water or an alcohol-water system, especially water, by a safe and simple process.
The invention takes the rubusoside as the carrier to improve the solubility of VD in water by 5 to 1200 times and improve the solubility of VE in water by 100 to 4.4 × 106And is stable for a long time.
Under proper conditions, the invention takes the rubusoside as a carrier, prepares fat-soluble vitamin particles which can form a colloid dispersion system or a colloid solution in a water phase by designing and selecting various process parameters and forming a colloid system, and is applied to water-based beverages and oral liquids. Of course, it can also be used in fat-soluble or emulsion type beverages or oral liquids. Due to the non-ionic property and the surface activity of the rubusoside, the rubusoside-vitamin system has good compatibility with a food system, and saccharides and proteins in the food further promote the formation of the colloid system and make the colloid system more stable.
The rubusoside is a safe sweetener used in food additive field, and has effects of lowering blood pressure, lowering blood sugar, resisting allergy, and inhibiting dental caries. The invention selects the rubusoside as a carrier, is applied to the preparation of VD and VE supplements, can achieve the effect of reducing blood sugar while supplementing VD and VE, is suitable for sugar-free functional foods and beverages required by diabetes patients, and has good application prospect.
Drawings
FIG. 1 shows the solubilizing effect of rubusoside at different concentrations on VE and VD.
FIG. 2 is a surface tension-concentration curve of rubusoside at different concentrations.
Detailed Description
The analysis method comprises the following steps:
(1) and (3) quantitatively detecting HP L C of VD and VE:
preparing VD and VE with different concentrations by using methanol, and detecting by using a high performance liquid chromatograph (diode array detector), wherein the detection conditions are that a Kromasil 100-5-C18 chromatographic column (4.6 × 250mm) is adopted, the column temperature is 30 ℃, acetonitrile is eluted at equal speed under the condition that the methanol is 75: 25(v/v), the sample introduction amount is 10 mu L, the flow rate is 1m L/min, the detection wavelength of VD is 265nm, and the detection wavelength of VE is 292nm, and standard curves of the concentrations of VD and VE and peak areas are respectively drawn.
(2) Solubility of vitamins in vitamin granules in water:
adding 10m L deionized water into a sample bottle, continuously adding vitamin particles, stirring at 25 ℃ until a small amount of solid is not dissolved, then continuously stirring for 60min, centrifuging, taking supernatant, filtering with a 0.22 mu m filter membrane, detecting with the high performance liquid chromatography condition, and calculating the solubility of VD and VE in water at 25 ℃ by a standard curve.
(3) Measurement of surface tension:
the surface tension of solutions of different concentrations of rubusoside (HP L C > 95% pure) at 25 ℃ was determined by drop volume method.
As shown in FIG. 1, 1% rubusoside can increase VE and VD respectively at room temperature2Solubility in Water 105And 111 times; the principle is not merely the solubilisation of hydrophobic regions in micelles, probably due to VE and VD2The unique weak surface activity enables the rubusoside to form similar co-micelles with the rubusoside or to be partially solubilized in a rubusoside fence, the CMC (see the attached figure 2 in the specification) of the rubusoside is remarkably increased, the solubility of VD in water can be improved by 5-1200 times under the temperature of 25 ℃, and the solubility of VE in water can be improved by 100-4.4 × 106Multiple times (see the attached figure 1a of the specification), and can be stable for a long time. Therefore, the method can prepare fat-soluble vitamin particles which can form a colloid dispersion system or a colloid solution in an aqueous phase by designing and selecting various process parameters and forming a colloid system under proper conditions by taking the rubusoside as a carrier, and can be applied to aqueous beverages and oral liquids.
Example 1 utilization ofThe purity is 95 percentThe rubusoside can be used for preparing VE granule and preparing black tea beverage
Dissolving 1g of 95% (mass purity) rubusoside in 35m L water at 20 ℃, stirring for 30min, dispersing 70mg of VE in 65m L30% ethanol water solution at 50 ℃ by using a homogenizer, stirring for 30min at 50 ℃, respectively obtaining a clear and transparent rubusoside solution and a uniformly dispersed VE suspension, slowly adding VE into the rubusoside solution under stirring at 50 ℃, stirring to obtain a rubusoside-VE solution, continuously stirring until the solution is clear and transparent, then continuously stirring for 30min, gradually cooling the solution to room temperature under stirring, carrying out reduced pressure rotary evaporation on the obtained rubusoside-VE solution at 30 ℃, carrying out vacuum drying to obtain a white solid, grinding the white solid, and sieving the white solid with a 200-mesh sieve to obtain powder, namely the VE particles which can be used in the beverage.
Through detection, the solubility of VE in the deionized water solution at 25 ℃ is 0.67mg/m L, and the vitamin E is 9.5 × 10 of the solubility of pure vitamin E in water4And (4) doubling.
The prepared vitamin E particles were added to commercially available bottled black tea beverages at mass concentrations of 4.0mg/m L and 5.0mg/m L, respectively, and left to stand at room temperature for 1 month without precipitation of solids.
Comparative example 1 useThe purity is 60 percentThe rubusoside can be used for preparing VE granule and preparing black tea beverage
Dissolving 1g of 60% rubusoside in 35m L water at 20 ℃, stirring for 30min, dispersing 70mg of VE in 65m L30% ethanol water solution at 50 ℃ by using a homogenizer, stirring for 30min at 50 ℃, respectively obtaining a clear and transparent rubusoside solution and a uniformly dispersed VE suspension, slowly adding the VE suspension into the rubusoside solution at 50 ℃, stirring to obtain a rubusoside-VE solution, continuously stirring until the solution is uniform and weak light bluish white, continuously stirring for 40min, gradually cooling the solution to room temperature under stirring, carrying out reduced pressure rotary evaporation on the obtained rubusoside-VE solution at 30 ℃, carrying out vacuum drying to obtain a white solid, and grinding the white solid through a 200-mesh sieve to obtain powder, namely the VE particles capable of being used in beverages.
It was found that the solubility of VE in deionized water solution at room temperature was 0.62mg/m L, which is 8 × 10% of the solubility of pure vitamin E in water4And (4) doubling.
The VE granules were added to commercial bottled black tea beverages at mass concentrations of 0.5mg/m L and 0.7mg/m L, respectively, and allowed to stand at room temperature for 1 month without solid precipitation.
Comparative example 2 95% rubusoside was directly mixed with VE
1g rubusoside with the purity of 95% and 70mg VE are directly mixed, and ground and sieved by a 200-mesh sieve to obtain white powder, namely VE granules containing rubusoside, and detection shows that the solubility of VE in deionized water solution at room temperature is 0.47mg/m L, which is 6.1 × 10 of the solubility of pure vitamin E in water4And (4) doubling.
Comparing the results of the present comparative example with those of example 1, it can be found that the solubilization of VE particles embedded with rubusoside micelles in example 1 has better solubility than the direct mixing of rubusoside and VE in the present comparative example.
Example 2 utilization ofThe purity is 95 percentThe rubusoside is used for assisting in dissolving and preparing VD particles and the VD particles are used for preparing the soymilk beverage
Dissolving 10g of 95% rubusoside in 10m L water at 85 ℃ to obtain a clear and transparent rubusoside solution, homogenizing 60mg of VD in 90m L20% ethanol water solution at 50 ℃ for 2min to obtain VD suspension, respectively stirring the rubusoside solutions at 85 ℃ for 30min, stirring the VD suspension at 50 ℃ for 30min, slowly adding the VD suspension into the rubusoside solution at 50 ℃ under stirring, mixing to obtain rubusoside-VD solution, continuously stirring until the solution is clear and transparent, continuously stirring for 30min, gradually cooling the solution to room temperature under stirring, carrying out rotary evaporation on the obtained rubusoside-VD solution at 25 ℃ and vacuum drying to obtain a white solid, grinding the white solid, and sieving the white solid with a 100-mesh sieve to obtain powder, namely VD particles capable of being used in beverages.
The room temperature solubility of VD in deionized water in the obtained particles is detected to be 0.51mg/m L, which is 1112 times of the solubility of pure vitamin D.
The VD granules were added to a commercially available soymilk beverage at a mass concentration of 0.5mg/m L and left to stand at room temperature for 1 month without solid precipitation.
Comparative example 3 uses a purity of60％The rubusoside is used for assisting in dissolving and preparing VD particles and the VD particles are used for preparing the soymilk beverage
Dissolving 10g of 60% rubusoside in 10m L water at 85 ℃, homogenizing 60mg of VD in 90m L20% ethanol water solution at 50 ℃ for 2min, stirring at respective mixing temperatures (85 ℃ and 50 ℃) for 40min to respectively obtain a clear and transparent rubusoside solution and a VD suspension, slowly adding the VD suspension into the rubusoside solution at 50 ℃ under stirring to obtain a rubusoside-VD solution, continuously stirring until the solution is uniform and weak light blue white, further stirring for 40min, then gradually cooling the solution to room temperature under stirring, carrying out rotary evaporation on the obtained rubusoside-VD solution at 25 ℃, carrying out vacuum drying to obtain a white solid, and grinding the white solid through a 100-mesh sieve to obtain powder which is VD particles capable of being used in beverages.
The room temperature solubility of VD in deionized water in the obtained particles is detected to be 0.45mg/m L, which is 1045 times of the solubility of pure vitamin D.
The VD granules were added to a commercially available soymilk beverage at a mass concentration of 0.07mg/m L and left to stand at room temperature for 1 month without solid precipitation.
Example 3 preparation of VE granules using 80% rubusoside co-dissolution and use of VE granules for the preparation of coffee beverages
Dissolving 0.5g of 80% rubusoside in 10m L water at 60 ℃, dispersing 5mg of VE in 90m 3515% ethanol water solution at 60 ℃ by using a homogenizer, stirring for 30min at corresponding dissolving or dispersing temperatures respectively to obtain a clear and transparent rubusoside solution and a uniformly dispersed VE suspension, slowly adding the VE suspension into the rubusoside solution at 60 ℃, stirring to obtain a rubusoside-VE solution, continuously stirring until the solution is uniform and weak light bluish white, continuously stirring for 40min, then gradually cooling the solution to room temperature under stirring, carrying out reduced pressure rotary evaporation on the obtained rubusoside-VE solution at 35 ℃, carrying out vacuum drying to obtain a white solid, grinding the white solid through a 100-mesh sieve, and obtaining powder which is VE particles capable of being used in beverages.
Through detection, the solubility of VE in the particle is 0.04mg/m L in deionized water solution at 25 ℃, which is 5600 times of the solubility of pure vitamin E in water.
The prepared vitamin E granules were added to a commercially available bottled coffee beverage at a mass concentration of 0.7mg/m L, and allowed to stand at room temperature for 1 month without precipitation of solids.
Example 4 preparation of VD particles using 80% rubusoside co-dissolution and use of VD particles for the preparation of sports energy beverages
Dissolving 0.5g of 80% rubusoside in 25m L water at 25 ℃, stirring for 40min, dispersing 2mg of VD in 75m L25% ethanol water solution at 50 ℃ by using a homogenizer, stirring for 30min, respectively obtaining clear and transparent rubusoside solution and VD suspension, slowly adding the VD suspension into the rubusoside solution at 50 ℃, mixing to obtain rubusoside-VD solution, continuously stirring until the solution is uniform and weak light blue white, further stirring for 40min, gradually cooling the solution to room temperature under stirring, vacuum drying the obtained rubusoside-VD solution at 55 ℃ to obtain white solid, and grinding the white solid through a 200-mesh sieve to obtain powder which is VD particles capable of being used in beverages.
The solubility of VD in the resulting particles was found to be 0.014mg/m L, which is 21 times the solubility of pure vitamin D, in deionized water at room temperature.
The VD particles are added into a certain commercially available kinetic energy beverage according to the mass concentration of 0.4mg/m L, and the beverage is kept stand for 1 month at room temperature, so that no solid is precipitated.
Example 5 preparation of VE granules using 95% rubusoside co-dissolution and use of VE granules for the preparation of fruit juice beverages
Dissolving 2g of 95% rubusoside in 20m L water at 60 ℃, stirring for 30min, dispersing 500mg of VE in 80m L20% ethanol water solution at 60 ℃ by using a homogenizer, stirring for 30min at corresponding dissolving or dispersing temperatures respectively to obtain clear and transparent rubusoside solution and uniformly dispersed VE suspension respectively, slowly adding the VE suspension into the rubusoside solution at 60 ℃, stirring to obtain rubusoside-VE solution, continuously stirring until the solution is uniform and weak light bluish white, continuously stirring for 30min, then gradually cooling the solution to room temperature under stirring, vacuum-drying the obtained solution at 35 ℃ to remove the solvent, freeze-drying to obtain white solid, and grinding the white solid through a 100-mesh sieve to obtain powder, namely VE particles capable of being used in beverages.
Example 6 preparation of VD granules using 95% rubusoside co-dissolution and use of VD granules for the preparation of juice beverages
Dissolving 2g of 95% rubusoside in 20m L water at 60 ℃, stirring for 40min, dispersing 10mg of VD in 80m L25% ethanol water solution at 50 ℃ by using a homogenizer, stirring for 30min, respectively obtaining clear and transparent rubusoside solution and VD suspension, slowly adding the VD suspension into the rubusoside solution at 50 ℃ under the stirring condition, mixing to obtain rubusoside-VD solution, continuously stirring until the solution is uniform and weak light blue white, further stirring for 30min, gradually cooling the solution to room temperature under stirring, vacuum drying the obtained rubusoside-VD solution at 25 ℃ under vacuum to remove the solvent, freeze-drying to obtain white solid, grinding the white solid through a 200-mesh sieve, and obtaining powder which is VD particles capable of being used in beverages.
The solubility of VD in the resulting particles was determined to be 0.081mg/m L, 188 times the solubility of pure vitamin D in deionized water at room temperature.
The VD particles were added to a commercially available fruit juice beverage at a mass concentration of 1mg/m L, and the mixture was allowed to stand at room temperature for 1 month without precipitation of solids.
Example 7 preparation of mixed VD-VE particles with 90% rubusoside co-dissolution and use of VD-VE particles for the preparation of a sports energy beverage
Dissolving 0.5g of 90% rubusoside in 35m L water at 85 ℃, stirring for 40min, dispersing 3mgVD and 2mgVE in 65m L30% ethanol water solution at 50 ℃ by using a homogenizer to respectively obtain a clear and transparent rubusoside solution and a VD-VE suspension, slowly adding the VD-VE suspension into the rubusoside solution at 50 ℃ under stirring to obtain a rubusoside-VD-VE solution, continuously stirring until the solution is uniform and weak light bluish white, further continuously stirring for 35min, then gradually cooling the solution to room temperature under stirring, vacuum drying the obtained rubusoside-VD-VE solution at 25 ℃ to obtain a white solid, grinding the white solid through a 200-mesh sieve, and obtaining powder which is the composite VE-VD particles capable of being used in beverages.
The vitamin complex particles are added into a certain commercially available kinetic energy beverage according to the mass concentration of 0.5mg/m L, and the beverage is kept standing at room temperature for 1 month, so that no solid is precipitated.
Example 8 preparation of VE granules using 90% rubusoside to aid dissolution and use of VE granules for the preparation of Zinc gluconate oral liquid
Dissolving 0.6g of 95% rubusoside in 50m L water at 90 ℃, stirring for 30min, dispersing 10mg of VE in 50 ℃ of 50m L40% ethanol water solution by using a homogenizer to respectively obtain clear and transparent rubusoside solution and uniformly dispersed VE suspension, slowly adding the VE suspension into the rubusoside solution under the stirring condition at 50 ℃, stirring to obtain rubusoside-VE solution, continuously stirring until the solution is clear and transparent, further stirring for 35min, gradually cooling the solution to room temperature under stirring, vacuum drying the obtained rubusoside-VE solution at 30 ℃ to obtain white solid, and grinding the white solid to obtain powder, namely the VE particles capable of being used in beverages.
The prepared VE granules are added into a commercial zinc gluconate oral liquid according to the mass concentration of 5.0mg/m L, and the mixture is kept stand at room temperature for 1 month, so that no solid is precipitated.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A process for preparing fat-soluble vitamin particles for use in beverages, comprising the steps of:
(1) dissolving rubusoside in solvent A at a temperature below 10 deg.C below the boiling point of solvent A, and stirring for 30-40min to obtain clear and transparent solution A; dispersing fat-soluble vitamins in solvent B by a homogenizer at the temperature of between room temperature and below 15 ℃ below the boiling point of the solvent B, and stirring for 30-40min to obtain uniformly dispersed suspension B;
(2) slowly adding the suspension B into the solution A under stirring at 30-60 ℃, mixing to obtain a solution C, continuously stirring the solution C until the solution is completely clear and transparent or is in a uniform and weak light blue white color, further continuously stirring at the same temperature for 30-40min, and then gradually cooling to room temperature under the stirring condition;
(3) drying the solution C obtained in the step 2 to obtain a white solid, grinding and sieving the white solid to obtain powder, namely fat-soluble vitamin particles which can be used in the beverage;
the solvent A is water, ethanol or an ethanol water solution, the solvent B is water, ethanol or an ethanol water solution, and the mass fraction of ethanol in the solution C is not more than 20%.
2. The method of claim 1, wherein the fat soluble vitamin is one of vitamin D or vitamin E, or a mixture of vitamin D and vitamin E.
3. The method of claim 1, wherein the purity of rubusoside expressed in HP L C is 60% or more.
4. A process for preparing fat-soluble vitamin granules usable in beverages according to claim 1 or 3, characterized in that the mass concentration of rubusoside in solution C is not less than 0.4%, said rubusoside being of vegetable origin or enzymatically synthesized.
5. A process for preparing fat-soluble vitamin granules usable in beverages according to claim 1, characterized in that the concentration by mass of vitamin E in solution C is not more than 1 × 10 of its solubility in the solvent of solution C5The mass concentration of the vitamin D is not more than 1000 times of the solubility of the vitamin D in the solvent of the solution C, and the solvent of the solution C is a mixed solvent consisting of the solvent A and the solvent B in the solution C.
6. A process for preparing fat-soluble vitamin granules useful in beverages according to claim 1, wherein said drying comprises freeze-drying, vacuum drying.
7. Fat-soluble vitamin particles for beverages prepared by the process according to any one of claims 1 to 8.
8. The use of the fat-soluble vitamin particles of claim 7 in aqueous, emulsion or oily oral liquids and beverages.
9. Application of rubusoside in preparing fat-soluble vitamin granule is provided.
10. Use of rubusoside as a co-solvent for vitamin E and/or vitamin D.
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