Vitamin B12 double-emulsion microcapsule and soft sweets containing vitamin B12 double-emulsion microcapsule

Through the dual emulsion microcapsule technology, vitamin B12 microcapsules were prepared by freeze-drying method of W1/O/W2 structure, which solved the problem of insufficient light stability during the storage process of vitamin B12 and achieved efficient storage stability of vitamin B12.

CN119563741APending Publication Date: 2025-03-07JIANGNAN UNIV +1

Patent Information

Application Number
CN202411670951.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-21
Publication Date
2025-03-07

AI Technical Summary

Technical Problem

Vitamin B12 is easily affected by light during the storage of gummy sugar and loses its activity, resulting in insufficient storage stability.

Method used

The dual emulsion microcapsule technology is used to prepare vitamin B12 microcapsules by freeze-drying method of W1/O/W2 structure, and the solid fat in the oil phase blocks ultraviolet rays and improves the light stability of vitamin B12.

Benefits of technology

It significantly improves the storage stability of vitamin B12, with an encapsulation rate of more than 65%. It can store it under room temperature light for 28 days, and the retention rate of vitamin B12 can reach more than 60%.

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Abstract

The invention discloses a preparation method of a double-emulsion microcapsule for improving the light stability of vitamin B12 in soft sweets. By constructing a double emulsion system, seepage of the vitamin B12 is effectively prevented, meanwhile, solid fat in an oil phase can effectively block damage of external ultraviolet rays to the vitamin B12, and the storage stability of the vitamin B12 is remarkably improved. In addition, the microcapsule is easy to disperse in water due to the selected water-soluble outer-layer wall material, so that the preparation of the soft sweets is facilitated. And the preparation process is simple and easy for large-scale production. The encapsulation efficiency of the vitamin B12 microcapsule prepared by the method is more than 65%. And the retention rate of the vitamin B12 can reach more than 60% after the vitamin B12 is stored for 28 days under a room-temperature illumination condition, which is obviously superior to the retention rate of the raw materials.
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Description

Technical Field

[0001] The invention belongs to the technical field of functional food processing, and in particular relates to a vitamin B12 double emulsion microcapsule and soft candy containing the vitamin B12 double emulsion microcapsule. Background Art

[0002] Vitamin B12, as a member of the B vitamins, is a water-soluble complex vitamin that mainly includes four forms: cyanocobalamin, hydroxocobalamin, methylcobalamin, and adenosylcobalamin. Among them, cyanocobalamin is the most stable and easily absorbed by the human body. Vitamin B12 plays multiple physiological roles in the human body, such as promoting the production of red blood cells, preventing pernicious anemia, maintaining the health of the nervous system, enhancing memory, and promoting DNA synthesis. Animal-derived foods, such as meat, eggs, and dairy products, are the main dietary sources of vitamin B12.

[0003] However, vegetarians and those with limited digestion and absorption capacity, such as pregnant women and the elderly, are often at risk of vitamin B12 deficiency. One of the common forms of vitamin B12 supplements on the market is multivitamin gummies. However, during the storage of gummies, vitamin B12 is easily affected by a variety of factors and loses its activity, especially the most significant effect of light. Therefore, it is particularly urgent to develop a method that can improve the photostability of vitamin B12 during the storage of gummies. Summary of the invention

[0004] The purpose of this section is to summarize some aspects of embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the specification abstract and the invention title of this application to avoid blurring the purpose of this section, the specification abstract and the invention title, and such simplifications or omissions cannot be used to limit the scope of the present invention.

[0005] In view of the above problems and / or the problems existing in the prior art, the present invention is proposed.

[0006] Therefore, the purpose of the present invention is to overcome the deficiencies in the prior art and provide a vitamin B12 double emulsion microcapsule.

[0007] In order to solve the above technical problems, the present invention provides the following technical solution: freeze-drying a double emulsion having a W1 / O / W2 structure, wherein:

[0008] W1 is the internal water phase, which is composed of vitamin B12 dissolved in sodium chloride aqueous solution;

[0009] O is the oil phase, which is composed of an emulsifier dissolved in a mixture of soybean oil and solid fat;

[0010] W2 is the external aqueous phase, which is composed of gum arabic, sodium caseinate, and xanthan gum dissolved in a sodium chloride aqueous solution;

[0011] The inner water phase W1 is dropped into the oil phase O and subjected to high-speed shearing to obtain a W1 / O emulsion, and the W1 / O emulsion is dropped into the outer water phase W2 and subjected to high-speed shearing to obtain a double emulsion with a W1 / O / W2 structure.

[0012] As a preferred embodiment of the vitamin B12 double emulsion microcapsule of the present invention, the concentration of the vitamin B12 in the inner water phase is 0.5-1.1 wt%.

[0013] As a preferred embodiment of the vitamin B12 double emulsion microcapsule of the present invention, the emulsifier is polyglycerol ricinoleate, and the concentration in the oil phase is 4-6 wt %;

[0014] The mass ratio of soybean oil to solid fat in the oil phase is 100:0 to 0:100.

[0015] As a preferred embodiment of the vitamin B12 double emulsion microcapsule of the present invention, in the external aqueous phase, the concentration of gum arabic is 5-15wt%, the concentration of sodium caseinate is 1-5wt%, and the concentration of xanthan gum is 0.1-0.5wt%.

[0016] As a preferred embodiment of the vitamin B12 double emulsion microcapsule of the present invention, the ratio of the inner water phase W1 to the oil phase O is 10:90 to 50:50.

[0017] As a preferred embodiment of the vitamin B12 double emulsion microcapsule of the present invention, the ratio of the W1 / O emulsion to the external water phase W2 is 5:95 to 30:70.

[0018] As a preferred embodiment of the vitamin B12 double emulsion microcapsule of the present invention, the high-speed shearing condition of the inner aqueous phase W1 dripping into the oil phase O is 12000rpm / 4min at 70°C; the high-speed shearing condition of the W1 / O emulsion dripping into the outer aqueous phase W2 is 76000rpm / 5min at 70°C.

[0019] As a preferred embodiment of the vitamin B12 double emulsion microcapsules of the present invention, the freeze-drying is performed by pre-freezing at -80°C for 8 hours, and then freeze-drying at -55°C and a vacuum degree of 5.9 Pa for 48 to 72 hours.

[0020] As a preferred embodiment of the vitamin B12 double emulsion microcapsules of the present invention, the encapsulation rate of the vitamin B12 microcapsules is greater than 65%, and the retention rate of the vitamin B12 is greater than 60% when stored at room temperature and under light conditions for 28 days.

[0021] Another object of the present invention is to provide a soft candy containing double emulsion microcapsules of vitamin B12.

[0022] In order to solve the above technical problems, the present invention provides the following technical solution: in terms of mass percentage of the soft candy, the raw materials include:

[0023] 0.002% to 1% of the vitamin B12 double emulsion microcapsule as claimed in claim 1, 72% to 74% of a sweetener, 2% to 3% of a colloid, 0.5% to 0.7% of a buffer salt, 0.3% to 0.4% of an acidity regulator, and the balance being water;

[0024] Wherein, the content of vitamin B12 in the vitamin B12 double emulsion microcapsule is 0.1% to 1%;

[0025] The sweetener is composed of white sugar, glucose syrup, and sorbitol solution with a mass fraction of 70%; the colloid includes pectin, the buffer salt includes one or more of anhydrous citric acid and sodium citrate, and the acidity regulator is citric acid solution with a mass fraction of 50%.

[0026] Another object of the present invention is to provide a method for preparing soft candy containing double emulsion microcapsules of vitamin B12.

[0027] In order to solve the above technical problems, the present invention provides the following technical solutions: comprising:

[0028] Pectin and white sugar are mixed in dry state, and 8 to 10 times of water are added to stir the solution to obtain a sugar-pectin solution;

[0029] The buffer salt is dissolved in water to obtain a buffer salt solution;

[0030] Add the sugar-pectin solution to the buffered saline solution, stirring continuously to avoid agglomeration, until a uniform mixed solution I without agglomeration is formed;

[0031] Add glucose syrup to the mixed solution I, stir and boil the sugar at 106-120° C. and 800 W electromagnetic power until the solid content reaches 75%, and cool to 65-70° C. to obtain a sugar solution;

[0032] After the vitamin B12 double emulsion microcapsules are dissolved in water, they are immersed in a 70% sorbitol solution at 40-45° C. to obtain a vitamin B12 solution;

[0033] The vitamin B12 solution is added to the sugar solution and stirred for 5 to 10 minutes to obtain a uniform jelly, to which 50% citric acid solution is added, and the mixture is cooled and dried to obtain soft candy containing double emulsion microcapsules of vitamin B12.

[0034] Beneficial effects of the present invention:

[0035] The present invention adopts microencapsulation technology to prepare vitamin B12 into a solid preparation. The double emulsion system effectively prevents the leakage of vitamin B12, and the solid fat in the oil phase can effectively block the damage of external ultraviolet rays to vitamin B12, thereby significantly improving the storage stability of vitamin B12. In addition, the water-soluble outer wall material selected by the present invention makes the microcapsules easy to disperse in water, which is convenient for the preparation of soft candies. The preparation process is simple and easy to scale up. The vitamin B12 microcapsules prepared by the method have an encapsulation rate of more than 65%. When stored under room temperature and light conditions for 28 days, the retention rate of vitamin B12 can reach more than 60%, which is significantly better than the retention rate of the raw material. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative labor. Among them:

[0037] Figure 1 This is the chromatogram of the vitamin B12 standard sample of the present invention. DETAILED DESCRIPTION

[0038] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the embodiments of the specification.

[0039] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein, and those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0040] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.

[0041] Unless otherwise specified, the raw materials used in the present invention are all commercially available in the art. Among them, the solid fat used is hydrogenated palm oil, model 1801, and the specific parameters are shown in Table 1.

[0042] Table 1

[0043] Chemical / physical properties scope Acid value, mgKOH / g 205-212 Saponification value, mgKOH / g 206-213 Iodine value, gI2 / 100g ≤0.3 Moisture content, %wt ≤0.3 Color, Lovibond 5% (Y / R) ≤3 / 0.3 Chroma ≤50 Freezing point, ℃ 54-56 C12: Lauric Acid ≤1 C14: Myristic acid ≤2 C16: Palmitic acid 54-62 C18:0: Stearic acid 37-43

[0044] The determination method of the vitamin B12 retention rate in the present invention is as follows:

[0045] 1. Preparation of Standard Solution

[0046] Vitamin B12 standard solutions (200, 400, 600, 800, 1000 ng / mL) were tested by high performance liquid chromatography to prepare a standard curve.

[0047] 2. Sample Solution Preparation

[0048] 2.1 Microcapsule pretreatment

[0049] Vitamin B12 on the surface of microcapsules: Weigh 0.05g of microcapsule powder (accurate to 0.01mg), disperse it in 20mL of pure water, fully dissolve, centrifuge (3000r / min, 5min) and take the supernatant. Take 1mL of the above liquid and dilute it to 20mL with pure water, filter it with a 0.22μm aqueous phase filter membrane, and inject it according to the chromatographic conditions.

[0050] Microcapsule total vitamin B12: Weigh 0.05g microcapsule powder (accurate to 0.01mg), disperse it in 20mL pure water, fully dissolve, and use an ultrasonic crusher to crush it, with an amplitude of 80%, a power of 130W, a pulse duration of 3s, a pause of 2s, and a total ultrasonic duration of 100s. Take 1mL of the above liquid and dilute it to 20mL with pure water, filter it with a 0.22μm aqueous phase filter membrane, and inject it according to chromatographic conditions.

[0051] 2.1 Pretreatment of soft candy

[0052] Weigh 5g of VB12 soft candy sample accurately (accurate to 0.0001g), add 10ml of pure water, stir until the soft candy is completely dissolved, and transfer to a 20ml volumetric flask to make up the volume. Pour into a 25ml beaker and use an ultrasonic crusher to crush it, with an amplitude of 80%, a power of 130W, a pulse duration of 3s, a stop of 2s, and a total ultrasonic duration of 100s. After cooling, centrifuge (12000r / min, 10min) to take the supernatant, filter through a 0.22μm microporous filter membrane, and inject according to chromatographic conditions.

[0053] 3. Chromatographic conditions

[0054] a) Chromatographic column: C18 column (column length 250mm×4.6mm×5μm)

[0055] b) Column temperature: 35°C

[0056] c) Mobile phase: 300 mL methanol + 700 mL water (1 g sodium hexane sulfonate + 690 mL water) + 10 mL acetic acid, vacuum filtration;

[0057] d) Flow rate: 1.0 mL / min

[0058] e) UV detection wavelength: 550nm

[0059] f) Injection volume: 20 μL

[0060] g) Retention time: 10min

[0061] h) Chromatogram: Figure 1 This is the peak chromatogram of B12 standard sample

[0062] 4. Analysis results and calculations

[0063] 4.1 Vitamin B12 content in microcapsule powder

[0064]

[0065] Where:

[0066] C——the concentration of vitamin B12 in the sample calculated according to the standard curve, in ng / mL;

[0067] 400——sample dilution multiple;

[0068] M sample - weighing of microcapsule powder, unit: g;

[0069] 4.2 Content of Vitamin B12 in Soft Candy Samples

[0070]

[0071] Where:

[0072] C——the concentration of vitamin B12 in the sample calculated according to the standard curve, in ng / mL;

[0073] 20——sample dilution multiple;

[0074] M sample: weight of soft candy, in g;

[0075] 4.3 The determination of the encapsulation rate of microcapsules vitamin B12 and the retention rate of vitamin B12 in soft candies is as follows:

[0076] Encapsulation efficiency = (1-X table / X total) × 100%;

[0077] Retention rate = (X G0 -X G ) / X G0 ×100%

[0078] Where:

[0079] X 表 - the vitamin B12 content on the microcapsule surface calculated in (a);

[0080] X 总 - the total vitamin B12 content of the microcapsules calculated according to (a);

[0081] X G0 - the initial vitamin B12 content of the soft candy calculated according to (b);

[0082] X G - the vitamin B12 content of the soft candy calculated according to (b);

[0083] Lighting experiment method reference:

[0084] The prepared vitamin B12 pectin gummies were placed in a 24-well plate and exposed to sunlight at room temperature for 4 weeks to measure the vitamin B12 retention rate.

[0085] Example 1

[0086] This embodiment provides a method for preparing vitamin B12 double emulsion microcapsules, specifically:

[0087] 1) Vitamin B12 is dissolved in a 150 mM NaCl aqueous solution to obtain an internal aqueous phase W1 having a vitamin B12 content of 1.1%;

[0088] 2) adding an emulsifier polyglycerol polyricinoleate (PGPR) to a mixture of soybean oil and hydrogenated palm oil in a ratio of 20:80, stirring at 70° C. for 30 min, to obtain an oil phase O with a PGPR content of 5%;

[0089] 3) The internal water phase W1 was preheated to 70°C and mixed with the oil phase O at a mass ratio of 1:1, and sheared at 12000 rpm at 70°C for 4 min to obtain a W1 / O emulsion;

[0090] 4) Arabic gum, sodium caseinate and xanthan gum are dissolved in a 150 mM NaCl aqueous solution to obtain an external aqueous phase W2 having an Arabic gum content of 15%, a sodium caseinate content of 2.5% and a xanthan gum content of 0.3%;

[0091] 5) W1 / O emulsion and W2 were mixed in a ratio of 10:90, and sheared at 70°C and 7600 rpm for 5 min to obtain W1 / O / W2 emulsion;

[0092] 6) The W1 / O / W2 emulsion was pre-frozen at -80°C for 8 hours and then freeze-dried for 60 hours. The condenser temperature was -55°C and the vacuum degree was 5.9 Pa to obtain the vitamin B12 double emulsion microcapsules of this example.

[0093] Example 2

[0094] The difference between this embodiment and embodiment 1 is that the ratio of soybean oil to hydrogenated palm oil in step 2) is adjusted to 0:100, and the remaining steps and processes are all referred to embodiment 1 to obtain the vitamin B12 double emulsion microcapsules of this embodiment.

[0095] Example 3

[0096] The difference between this embodiment and embodiment 1 is that the ratio of soybean oil to hydrogenated palm oil in step 2) is adjusted to 40:60, and the remaining steps and processes are all referred to embodiment 1 to obtain the vitamin B12 double emulsion microcapsules of this embodiment.

[0097] Example 4

[0098] The difference between this embodiment and embodiment 1 is that the ratio of soybean oil to hydrogenated palm oil in step 2) is adjusted to 60:40, and the remaining steps and processes are all based on embodiment 1 to obtain the vitamin B12 double emulsion microcapsules of this embodiment.

[0099] Example 5

[0100] The difference between this embodiment and embodiment 1 is that the ratio of soybean oil to hydrogenated palm oil in step 2) is adjusted to 80:20, and the remaining steps and processes are all referred to embodiment 1 to obtain the vitamin B12 double emulsion microcapsules of this embodiment.

[0101] Example 6

[0102] The difference between this embodiment and embodiment 1 is that the ratio of soybean oil to hydrogenated palm oil in step 2) is adjusted to 100:0, and the remaining steps and processes are all referred to embodiment 1 to obtain the vitamin B12 double emulsion microcapsules of this embodiment.

[0103] Comparative Example 1

[0104] This comparative example is different from Example 1 in that an oil-free vitamin B12 microcapsule is provided, specifically:

[0105] 1) Vitamin B12 is dissolved in a 150 mM NaCl aqueous solution to obtain an internal aqueous phase W1 having a vitamin B12 content of 1.1%;

[0106] 2) Gum arabic, sodium caseinate and xanthan gum are dissolved in a 150 mM NaCl aqueous solution to obtain an external aqueous phase W2 having a gum arabic content of 15%, a sodium caseinate content of 2.5% and a xanthan gum content of 0.3%; and

[0107] 3) W1 and W2 were mixed at a ratio of 4:96, and magnetically stirred at 600 rpm for 3 min to obtain a W1W2 two-phase mixed solution;

[0108] 4) The W1W2 two-phase mixed solution was pre-frozen at -80°C for 8 hours, and then freeze-dried for 60 hours. The condenser temperature was -55°C and the vacuum degree was 5.9 Pa, thereby obtaining the oil-free vitamin B12 microcapsules of this comparative example.

[0109] Application Testing

[0110] In order to verify the protective effect of the vitamin B12 double emulsion microcapsules prepared by the present invention on vitamin B12, the microcapsules were prepared into soft candies, specifically:

[0111] 1) Weigh the raw materials according to the pectin soft candy formula in Table 1:

[0112] Table 1 Pectin Soft Candy Formula

[0113]

[0114] 2) Preparation of soft candy:

[0115] Pectin and white sugar were first mixed in dry state, and 10 times of water was added to dissolve at 80°C and 600 rpm for 10 minutes to obtain a sugar-pectin solution;

[0116] Take an empty pot and a spatula, add weighed sodium citrate, citric acid and about 30g of pure water, and cook at 65℃ (1st gear 400W on an induction cooker) for 5min to obtain a buffered salt solution;

[0117] Add the sugar-pectin solution to the buffered saline solution, stirring continuously to avoid agglomeration, until a uniform mixed solution I without agglomeration is formed;

[0118] Add glucose syrup to the mixed solution I, stir and boil the sugar at 120°C and 800W electromagnetic power until the solid content reaches 75%, and cool to 70°C to obtain a sugar solution;

[0119] Vitamin B12 microcapsules were dissolved in 50 g pure water by stirring, immersed in 70% sorbitol solution at 4°C for 5 min, added to the sugar solution and stirred for 10 min to obtain a uniform jelly, to which 50% citric acid solution was added and stirred for 2 min. After cooling, the jelly was dried in an oven at 35°C for 24 h to obtain soft candies containing vitamin B12 in different forms. Relevant performance tests were carried out, and the results are shown in Table 2.

[0120] Table 2

[0121]

[0122] As can be seen from the table above, the retention rate of vitamin B12 in the soft candy of the microcapsules without oil phase is higher than that of the pure vitamin B12 powder. This may be because the macromolecular protein and pectin in the external water phase can bind to vitamin B12, thereby providing a certain UV shielding effect. However, due to the relatively weak binding ability, the encapsulation rate is low, and thus the retention rate is also relatively low. With the addition of the oil phase, the encapsulation rate is significantly improved, which allows more vitamin B12 to be encapsulated in the wall material and improves the retention rate.

[0123] Compared with soybean oil, solid hydrogenated palm oil exhibits stronger UV shielding ability. As the solid fat content in the oil phase increases, it can form a denser UV shielding layer, thereby further improving the retention rate of vitamin B12. However, too high a solid fat content may cause vitamin B12 to leak from the inner water phase, affecting its protective effect, and may reduce the solubility of the powder in water. This requires greater stress to promote the dissolution process, which may lead to a decrease in encapsulation efficiency and ultimately affect the retention rate.

[0124] Example 6

[0125] This example is used to explore the effect of different W1 / O emulsions compared with W2 on the light retention rate of the prepared vitamin B12 microcapsules, specifically:

[0126] The difference from Example 1 is that the ratio of W1 / O emulsion to W2 is adjusted to 5:95, 10:90, 15:85, 20:80, and 25:75, respectively, to obtain vitamin B12 microcapsules with different W1 / O emulsions to W2 in this example, and soft candies are prepared according to the above method, and relevant properties are measured. The results are shown in Table 3.

[0127] Table 3

[0128]

[0129] As can be seen from the above table, as the W1 / O phase ratio increases, the average particle size of the microcapsules decreases, which leads to an increase in their specific surface area. This reduction in particle size may reduce the contact area between vitamin B12 and light, thereby helping to improve the retention rate of vitamin B12 under light conditions. However, the increase in the W1 / O phase ratio also leads to an increase in the drug loading of the microcapsules, and a corresponding decrease in the relative content of the wall material in the W2 phase, which may weaken the encapsulation rate and ultraviolet light shielding effect of the microcapsules. Therefore, a balanced ratio is required. When W1 / O:W2=10:90, the photostability of vitamin B12 can be improved while maintaining sufficient encapsulation rate and ultraviolet light shielding effect.

[0130] Example 7

[0131] This example is used to explore the effect of different contents of gum arabic in the external aqueous phase W2 on the light retention rate of the prepared vitamin B12 microcapsules, specifically:

[0132] The contents of gum arabic in the external aqueous phase W2 of Example 1 were adjusted to 0, 5, 10, 15, and 20%, respectively, to obtain vitamin B12 microcapsules with different contents of gum arabic in this example. Soft candies were prepared according to the above method, and relevant properties were measured. The results are shown in Table 4.

[0133] Table 4

[0134]

[0135] As can be seen from the table above, with the increase of the content of the excipient gum arabic, its solubility in the powder has been significantly improved, and the encapsulation rate and retention rate of the microcapsules have also increased. However, the increase in the excipient content will also lead to a decrease in the particle size of the microcapsules and an increase in the specific surface area, which will increase the light contact area of ​​vitamin B12, which may lead to a decrease in the retention rate of vitamin B12 under light conditions. Therefore, when the content of gum arabic is set to 15%, the best effect can be obtained.

[0136] Example 8

[0137] This example is used to explore the effect of different sodium caseinate contents in the external aqueous phase W2 on the light retention rate of the prepared vitamin B12 microcapsules, specifically:

[0138] The contents of sodium caseinate in the external aqueous phase W2 of Example 1 were adjusted to 1.5, 2, 2.5, 3, and 3.5%, respectively, to obtain vitamin B12 microcapsules with different casein contents in this example. Soft candies were prepared according to the above method, and relevant properties were measured. The results are shown in Table 5.

[0139] Table 5

[0140]

[0141]

[0142] According to the above results, with the increase of sodium caseinate content, the emulsification ability of the W / O / W system is enhanced, which leads to an increase in the encapsulation rate of the microcapsules, resulting in better light stability and higher vitamin B12 retention rate. The tyrosine and tryptophan residues in sodium caseinate contain benzene ring structures. These structures show strong ultraviolet absorption peaks at a wavelength of 280nm due to the presence of conjugated double bonds, providing a certain ultraviolet shielding effect for the microcapsules. However, when the content of sodium caseinate continues to increase, the film-forming property of the wall material will decrease, thereby weakening the stability of the wall material, which may cause the light stability of the microcapsules to decrease again. Therefore, 3% is the optimal content of sodium caseinate. After exceeding this content, the performance of the microcapsules will be affected.

[0143] Comparative Example 2

[0144] This example is used to explore the effects of different types of oil phase emulsifiers on the light retention rate of the prepared vitamin B12 microcapsules, specifically:

[0145] The type of oil phase emulsifier (PGPR, phospholipid) in Example 1 was adjusted to obtain vitamin B12 microcapsules with different contents of gum arabic in this example. Soft candies were prepared according to the above method, and relevant properties were measured. The results are shown in Table 6.

[0146] Table 6

[0147]

[0148] According to the above results, the use of PGPR as an emulsifier has a higher encapsulation rate, which can prevent the leakage of vitamin B12 and fully encapsulate it in the microcapsules. Compared with phospholipids, PGPR has a stronger water encapsulation ability when used as an emulsifier. This is because PGPR can not only stabilize W / O emulsions, but also produce a synergistic effect with other ingredients such as sodium caseinate, further reducing the interfacial tension and enhancing the stability of the emulsion.

[0149] In summary, the present invention adopts microencapsulation technology to make vitamin B12 into a solid preparation. The double emulsion system can effectively prevent the leakage of vitamin B12, and the solid fat in the oil phase can effectively block the damage of external ultraviolet rays to vitamin B12, significantly improving the storage stability of vitamin B12. In addition, the water-soluble outer wall material selected by the present invention makes the microcapsules easy to disperse in water, which is convenient for the preparation of soft candies. The preparation process is simple and easy to scale production. The vitamin B12 microcapsules prepared by this method have an encapsulation rate of more than 65%. After being stored for 28 days under room temperature and light conditions, the retention rate of vitamin B12 can reach more than 60%, which is significantly better than the retention rate of the raw material.

[0150] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.

Claims

1. A vitamin B12 double emulsion microcapsule, characterized in that: It is obtained by freeze-drying a double emulsion with a W1 / O / W2 structure, wherein: W1 is the internal water phase, which is composed of vitamin B12 dissolved in sodium chloride aqueous solution; O is the oil phase, which is composed of an emulsifier dissolved in a mixture of soybean oil and solid fat; W2 is the external water phase, which is composed of gum arabic, sodium caseinate, and xanthan gum dissolved in a sodium chloride aqueous solution; The inner water phase W1 is dropped into the oil phase O and subjected to high-speed shearing to obtain a W1 / O emulsion, and the W1 / O emulsion is dropped into the outer water phase W2 and subjected to high-speed shearing to obtain a double emulsion with a W1 / O / W2 structure.

2. The vitamin B12 double emulsion microcapsule according to claim 1, characterized in that: The concentration of the vitamin B12 in the internal water phase is 0.5-1.1 wt %. The vitamin B12 double emulsion microcapsule according to claim 1, characterized in that the emulsifier is polyglycerol ricinoleate, and the concentration in the oil phase is 4 to 6 wt%.

3. The vitamin B12 double emulsion microcapsule according to claim 1, characterized in that: In the external water phase, the concentration of gum arabic is 5-15wt%, the concentration of sodium caseinate is 1-5wt%, and the concentration of xanthan gum is 0.1-0.5wt%.

4. The vitamin B12 double emulsion microcapsule according to claim 2, characterized in that: The ratio of the internal water phase W1 to the oil phase O is 10:90 to 50:

50.

5. The vitamin B12 double emulsion microcapsule according to claim 1, characterized in that: The ratio of the W1 / O emulsion to the external water phase W2 is 5:95 to 30:

70.

6. The vitamin B12 double emulsion microcapsule according to claim 1, characterized in that: The high-speed shearing condition for the inner water phase W1 to be dripped into the oil phase O is 12000 rpm / 4 min at 70°C; the high-speed shearing condition for the W1 / O emulsion to be dripped into the outer water phase W2 is 76000 rpm / 5 min at 70°C.

7. The vitamin B12 double emulsion microcapsule according to claim 1, characterized in that: The freeze drying is performed by pre-freezing at -80°C for 8 hours, and then freeze drying at -55°C and a vacuum degree of 5.9 Pa for 48 to 72 hours.

8. The double emulsion microcapsule containing vitamin B12 according to any one of claims 1 to 7, characterized in that: The encapsulation rate of the vitamin B12 microcapsules is greater than 65%, and the retention rate of the vitamin B12 is greater than 60% when stored at room temperature and under light conditions for 28 days.

9. A soft candy containing double emulsion microcapsules of vitamin B12, characterized in that: Calculated by mass percentage of the soft candy, the raw materials include: 0.002% to 1% of the vitamin B12 double emulsion microcapsule as claimed in claim 1, 72% to 74% of a sweetener, 2% to 3% of a colloid, 0.5% to 0.7% of a buffer salt, 0.3% to 0.4% of an acidity regulator, and the balance being water; Wherein, the content of vitamin B12 in the vitamin B12 double emulsion microcapsule is 0.1% to 1%; The sweetener is composed of white sugar, glucose syrup, and sorbitol solution with a mass fraction of 70%; the colloid includes pectin, the buffer salt includes one or more of anhydrous citric acid and sodium citrate, and the acidity regulator is citric acid solution with a mass fraction of 50%.

10. The method for preparing soft candy containing double emulsion microcapsules of vitamin B12 according to claim 9, characterized in that: include, Pectin and white sugar are mixed in dry state, and 8 to 10 times of water are added to stir the solution to obtain a sugar-pectin solution; The buffer salt is dissolved in water to obtain a buffer salt solution; Add the sugar-pectin solution to the buffered saline solution, stirring continuously to avoid agglomeration, until a uniform mixed solution I without agglomeration is formed; Add glucose syrup to the mixed solution I, stir and boil the sugar at 106-120° C. and 800 W electromagnetic power until the solid content reaches 75%, and cool to 65-70° C. to obtain a sugar solution; After the vitamin B12 double emulsion microcapsules are dissolved in water, they are immersed in a 70% sorbitol solution at 40-45° C. to obtain a vitamin B12 solution; The vitamin B12 solution is added to the sugar solution and stirred for 5 to 10 minutes to obtain a uniform jelly, to which 50% citric acid solution is added, and the mixture is cooled and dried to obtain soft candy containing double emulsion microcapsules of vitamin B12.

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