High-steady-state vitamin B1 micro-capsule powder applied to soft capsules and preparation method of high-steady-state vitamin B1 micro-capsule powder

Abstract

The invention discloses high-steady-state vitamin B1 micro-capsule powder applied to soft capsules and a preparation method. The micro-capsule powder is prepared from the following raw materials in parts by weight: 10-65 parts of a vitamin B1 core material, 10-30 parts of a wall material, 0.5-2 parts of a small molecular emulsifier and 5-35 parts of a filler, the wall material is prepared from starch sodium octenylsuccinate and pectin in a mass ratio of (1.5-5): 1; and the mass ratio of the wall material to the core material is not greater than 1: 2.3. Compared with the prior art, the vitamin B1 microcapsule powder prepared by the invention can effectively delay degradation of vitamin B1 in soft capsules and solve the problem that the vitamin B1 soft capsules are unstable within the shelf life, has higher stability in the soft capsules, meanwhile, the loading capacity of effective components is higher, and the production efficiency is greatly improved.

Description

Technical Field

[0001] The invention belongs to the technical field of food processing, and in particular relates to a high-stable vitamin B1 microcapsule powder used in soft capsules and a preparation method thereof. Background Art

[0002] Vitamin B1, as the earliest water-soluble vitamin extracted and purified, has the function of maintaining normal sugar metabolism and nerve conduction, and is widely used in the field of health foods. However, vitamin B1 has a weak peculiar smell, bitter taste, deliquescent, heat-resistant, very unstable under neutral and acidic conditions, and easily oxidized and inactivated. At present, the dosage forms of health foods supplementing vitamin B1 include tablets, oral liquids, capsules, etc. Compared with other dosage forms, soft capsules have the advantages of high bioavailability and good stability. They are suitable for nutrients with bad odor, unstable in light, heat, and moisture, and easily oxidized, and can effectively mask the bitter taste of vitamin B1. However, since the capsule shell of the soft capsule usually contains a certain amount of water, there will be some stability problems, such as the phenomenon of material migration in the capsule during storage, including the migration of water in the capsule shell to the contents, or the migration of the contents to the capsule shell, which will cause the degradation and loss of nutrients.

[0003] At present, the prior art publicly uses hydrophilic colloids such as carboxymethyl cellulose, gelatin or xanthan gum to process complex B vitamins through microencapsulation, which effectively improves the light and heat stability of B vitamins. There are also studies that use multiple emulsification-complex coacervation technology to microencapsulate vitamin B1, which has a good protective effect on vitamin B1. However, it does not solve the problem of vitamin B1 degradation in soft capsule dosage forms. In addition, a large amount of high-viscosity colloidal substances are used in the preparation method, which not only has a low content of effective substances, but also has a very high viscosity of the overall solution, and there is also a problem of low production efficiency. Summary of the invention

[0004] The purpose of the present invention is to provide a highly stable vitamin B1 microcapsule powder for soft capsules and a preparation method thereof in order to solve the deficiencies of the prior art.

[0005] The purpose of the present invention is achieved by the following technical solutions:

[0006] A highly stable vitamin B1 microcapsule powder for soft capsules is prepared from the following raw materials in parts by weight: 10 to 65 parts of a vitamin B1 core material, 10 to 30 parts of a wall material, 0.5 to 2 parts of a small molecule emulsifier, and 5 to 35 parts of a filler;

[0007] The wall material is composed of sodium starch octenyl succinate and pectin in a mass ratio of (1.5-5):1; the mass ratio of the wall material to the core material is not greater than 1:2.3.

[0008] Preferably, the molecular weight of the small molecule emulsifier is not greater than 1000.

[0009] Preferably, the small molecule emulsifier is mono- and di-glycerol fatty acid ester and / or sucrose fatty acid ester.

[0010] Preferably, the filler is maltodextrin.

[0011] The method for preparing the high-stable vitamin B1 microcapsule powder for soft capsules as described above comprises the following steps:

[0012] S1. First, the wall material and the filler are dissolved to prepare a wall material solution;

[0013] S2. The pH of the wall material solution is adjusted to 5-6, vitamin B1 and a small molecule emulsifier are added, and then high-speed shearing is performed to fully emulsify the solution;

[0014] S3. Then spray drying is performed to obtain microcapsule powder.

[0015] Preferably, the dissolving temperature in step S1 is 65-85°C.

[0016] Preferably, the shear rate in step S2 is 6000-10000 r / min, and the shear time is 5-10 min.

[0017] Preferably, the spray drying parameters are:

[0018] The inlet air temperature is 160~180℃ and the outlet air temperature is 90~100℃.

[0019] Preferably, the atomizer frequency is 300-360 Hz.

[0020] Preferably, after drying in step S3, the product further includes passing through a 80-120 mesh sieve.

[0021] Compared with the prior art, the vitamin B1 microcapsule powder prepared in the present application can effectively delay the degradation of vitamin B1 in soft capsules, solve the problem of instability of vitamin B1 soft capsules during the shelf life, has higher stability in soft capsules, and at the same time has a higher active ingredient load, greatly improving production efficiency. DETAILED DESCRIPTION

[0022] The invention provides a high-stable vitamin B1 microcapsule powder for soft capsules, which is prepared from the following raw materials in parts by weight: 10 to 65 parts of a vitamin B1 core material, 10 to 30 parts of a wall material, 0.5 to 2 parts of a small molecule emulsifier and 5 to 35 parts of a filler; the mass ratio of the wall material to the core material is not greater than 1:2.3; the wall material is composed of sodium starch octenyl succinate and pectin in a mass ratio of (1.5 to 5):1; the molecular weight of the small molecule emulsifier is generally not greater than 1000.

[0023] The present application adopts biopolymer film embedding technology, uses sodium starch octenylsuccinate as the main wall material, compound pectin, and adds small molecule emulsifiers and fillers to prepare vitamin B1 microcapsule powder suitable for soft capsules.

[0024] Among them, sodium starch octenyl succinate has the characteristics of low viscosity and high film-forming property. It can quickly condense and solidify on the surface of the core material to form a dense film during the drying process. At the same time, sodium starch octenyl succinate contains certain octenyl succinate groups, which have lipophilic characteristics and can increase the solubility of vitamin B1 in oils and fats, thereby improving the lipophilicity of microcapsule powder, avoiding soft capsule stratification, reducing the migration of contents in soft capsules to the soft capsule shell, and improving the stability of vitamin B1 in soft capsules. Pectin is a natural hydrophilic colloid with good emulsification, solubility and fluidity. When used in combination with sodium starch octenyl succinate, it can increase the toughness of the capsule wall and effectively avoid cracks in the capsule wall caused by rapid migration of water during the drying process. The combination of the two can form a more complete spherical microcapsule. In addition, sodium octenyl succinate starch and pectin are also macromolecular emulsifiers, and their arrangement on the interface is not compact enough. Therefore, the present invention adds a certain amount of small molecule emulsifier, which can be adsorbed on the interface faster to form uniform emulsion droplets. On the one hand, it can avoid the droplet flocculation phenomenon when the sodium octenyl succinate starch concentration is high, improve the stability of the system, and enable it to maintain a smaller particle size. On the other hand, as a small molecule emulsifier, it can reduce the interfacial tension between the two phases, change the charge distribution on the droplet surface, and maintain a stronger electrostatic repulsion between the droplets, thereby improving its stability. The filler can reduce the crystallization rate of the core material, increase the glass transition temperature of the composition, and enable it to have a faster drying rate in the subsequent spray drying process, forming a fuller capsule wall and improving the powder yield.

[0025] Compared with the prior art, the vitamin B1 microcapsule powder prepared in the present application can effectively delay the degradation of vitamin B1 in soft capsules, solve the problem of instability of vitamin B1 soft capsules during the shelf life, has higher stability in soft capsules, and at the same time has a higher active ingredient load, greatly improving production efficiency.

[0026] Preferably, the small molecule emulsifier is mono- and di-glycerol fatty acid ester and / or sucrose fatty acid ester.

[0027] Preferably, the bulking agent is maltodextrin.

[0028] Mono- and di-glycerol fatty acid esters and sucrose fatty acid esters can balance water and oil well and reduce the HLB value of the composite wall material; maltodextrin as a filler has a higher glass transition temperature and increases the powder yield.

[0029] As mentioned above, sodium octenyl succinate starch as the main wall material has the characteristics of rapid film formation, but it is easy to form cracks during the drying process, especially during the spray rapid drying process. Experiments have shown that compounding an appropriate amount of hydrophilic colloid pectin can significantly improve the fluidity and integrity of the film, and the surface modification of small molecule emulsifiers can further improve the stability of microcapsule droplets. There is a synergistic effect between the components, and the ratio between the raw materials has an important influence on the quality of the product. This application optimizes the formula based on the loss of vitamin B1 in the production process as an indicator, as follows:

[0030] Firstly, an optimization experiment was conducted on the ratio of sodium starch octenyl succinate and pectin. The experimental conditions were as follows: the proportion of vitamin B1 was fixed at 60%; maltodextrin was used as the filler, accounting for 10%; sucrose fatty acid ester was used as the small molecule emulsifier, accounting for 2%; the proportion of wall material was fixed at 28%. Sodium starch octenyl succinate and pectin with different mass ratios were used to prepare microcapsule powder under the same production conditions, and the content of vitamin B1 in the obtained microcapsule powder was detected. The results are shown in Table 1.

[0031] Table 1

[0032]

[0033] As can be seen from Table 1, when the mass ratio of sodium starch octenyl succinate to pectin is between 8:2 and 6:4, that is, when sodium starch octenyl succinate is used as the main wall material, the product has the highest vitamin B1 content and the vitamin B1 loss is within 1%.

[0034] When the mass ratio of sodium starch octenyl succinate to pectin is 7:3, the loss of vitamin B1 is minimal, so the mass ratio of sodium starch octenyl succinate to pectin is further preferably 7:3.

[0035] Then, an optimization experiment was carried out on the wall-core ratio. The experimental conditions were as follows: the composite wall material was prepared with sodium starch octenylsuccinate and pectin in a mass ratio of 7:3, sucrose fatty acid ester was selected as the small molecule emulsifier, accounting for 2%, and maltodextrin was selected as the filler, accounting for 28%. Microcapsule powders were prepared under the same production conditions with different mass ratios of wall-core ratios, and the content of vitamin B1 in the obtained microcapsule powders was detected. The results are shown in Table 2.

[0036] Table 2

[0037]

[0038] It can be seen from Table 2 that when the wall-core ratio is within 1:2.3, the loss of vitamins is less. Therefore, the wall-core ratio is limited to no more than 1:2.3, and further limited to 1:2.

[0039] Finally, an optimization experiment was conducted on the proportion of small molecule emulsifiers. The experimental conditions were: the proportion of vitamin B1 was fixed at 56%, the proportion of wall materials was fixed at 28%, sucrose fatty acid ester was used as the small molecule emulsifier, and different addition ratios were selected. The remainder was filler. Maltodextrin was used as the filler. Microcapsule powder was prepared under the same production conditions, and the content of vitamin B1 in the obtained microcapsule powder was detected. The results are shown in Table 3.

[0040] Table 3

[0041]

[0042] It can be seen from Table 3 that when the proportion of small molecule emulsifier is within 0.5-2%, the vitamin B1 content in the product is the highest, so the amount of small molecule emulsifier is limited to 0.5-2%, and more preferably 1%.

[0043] The present application also provides a method for preparing the high-stable-state vitamin B1 microcapsule powder for soft capsules as described above, comprising the following steps:

[0044] S1. First, the wall material and the filler are dissolved in water to prepare a wall material solution; the dissolution temperature is preferably 65 to 85 ° C, which can accelerate the dissolution and improve the uniformity of the raw material dissolution; the solid content of the wall material solution is preferably 10 to 20%;

[0045] S2. The pH of the wall material solution is adjusted to 5-6, vitamin B1 and a small molecule emulsifier are added, and then high-speed shearing is performed to fully emulsify the solution; firstly, the pH of the solution is adjusted to 5-6, so that the wall material is in the most suitable emulsification condition and the microcapsules are formed better; preferably, the shear rate is 6000-10000 r / min, and the shear time is 5-10 min, within which range the solution can be fully sheared and emulsified; the pH adjusting agent is preferably citric acid and sodium citrate, which are used as pH adjusting agents with higher safety;

[0046] S3. Then spray drying is performed to obtain microcapsule powder. Spray drying has a fast rate and less loss of nutrients, so this application uses spray drying to prepare microcapsule powder. Spray drying parameters are preferably: inlet air temperature 160-180°C, outlet air temperature 90-100°C, and atomizer frequency 300-360Hz. The use of these parameters can minimize the loss of nutrients and avoid cracks caused by sodium starch octenyl succinate.

[0047] Preferably, after drying, the powder is screened through a sieve of 80 to 120 meshes to remove large particles and improve the uniformity of the microcapsule powder.

[0048] After obtaining the microcapsule powder, it is added to conventional soft capsule materials in a certain proportion, and vitamin B1 soft capsules can be prepared according to conventional methods. Through the optimization of the vitamin B1 microcapsule powder formula and preparation process in this application, the degradation of nutrients in the soft capsules can be avoided, and the obtained vitamin B1 soft capsules have strong stability and less vitamin B1 loss.

[0049] Example 1

[0050] The microcapsule powder formula is: 60% vitamin B1, 21.0% sodium starch octenyl succinate, 9.0% pectin, 2.0% sucrose fatty acid ester (molecular weight 627), 8.0% maltodextrin, and the microcapsule powder is prepared by the following method.

[0051] (1) using a purified aqueous solution at 75° C. as a solvent, adding sodium starch octenyl succinate, pectin and maltodextrin, and stirring until completely dissolved and dispersed to prepare a wall material solution with a solid content of 15%;

[0052] (2) After the wall material solution is cooled to room temperature, citric acid and sodium citrate are used to adjust the solution pH to 5.5, and then vitamin B1 is added. After sufficient stirring to dissolve, sucrose fatty acid ester is added and sheared and homogenized at 8000 r / min for 8 minutes using a high-speed shearing machine to fully emulsify the solution;

[0053] (3) The emulsified solution was dried using a spray dryer. The spray dryer was set with an inlet air temperature of 170°C, an outlet air temperature of 95°C, and an atomizer frequency of 330 Hz. When the inlet and outlet air temperatures reached the set values, spray drying began. The collected material was sieved through a 100-mesh national standard sieve to obtain vitamin B1 microcapsule powder.

[0054] Then the microcapsule powder was filled into soft capsules to prepare soft capsules with a vitamin B1 content of 15%. The soft capsules were placed in an accelerated test chamber at 37° C. and 75% relative humidity for stability testing. The results are shown in Table 5.

[0055] Different formulations were selected for comparative experiments. The formulations are shown in Table 4. The production conditions were the same as in Example 1. The results are shown in Table 5.

[0056] Table 4 Example and Comparative Example Formula Design

[0057]

[0058] Table 5

[0059]

[0060] As can be seen from Table 5, after 3 months of accelerated storage, the vitamin B1 loss rate of Examples 1 to 4 using the formula of the present application is still less than 10%, while the vitamin B1 loss rate of Comparative Example 1 without adding pectin is as high as 65%, the vitamin B1 loss rate of not adding sodium octenyl succinate starch is as high as 61%, and the vitamin B1 loss rate of not adding small molecule emulsifier is also 36%. The stability of the soft capsules obtained in the present application is greatly improved compared with the comparative examples, which proves that the above-mentioned raw materials are indispensable and the components have a synergistic effect, which further fully proves that the technical solution of the present invention has the effect of solving the degradation of vitamin B1 in soft capsules.

[0061] Although preferred embodiments of the present invention have been described, additional changes and modifications may be made to these embodiments by those skilled in the art once the basic inventive concepts are known. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the present invention. Obviously, those skilled in the art may make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

Claims

1. A highly stable vitamin B1 microcapsule powder for soft capsules, characterized in that: The invention is prepared from the following raw materials in parts by weight: 10 to 65 parts of vitamin B1 core material, 10 to 30 parts of wall material, 0.5 to 2 parts of small molecule emulsifier and 5 to 35 parts of filler; The wall material is composed of sodium starch octenyl succinate and pectin in a mass ratio of (1.5-5):1; the mass ratio of the wall material to the core material is not greater than 1:2.

3.

2. The high-stable vitamin B1 microcapsule powder for soft capsules according to claim 1, characterized in that: The molecular weight of the small molecule emulsifier is not greater than 1000.

3. The high stable vitamin B1 microcapsule powder for soft capsules according to claim 1, characterized in that: The small molecule emulsifier is mono- and di-glycerol fatty acid ester and / or sucrose fatty acid ester.

4. The high-stable vitamin B1 microcapsule powder for soft capsules according to claim 1, characterized in that: The filler is maltodextrin.

5. The method for preparing the highly stable vitamin B1 microcapsule powder for soft capsules according to any one of claims 1 to 4, characterized in that: The following steps are involved: S1. First, the wall material and the filler are dissolved to prepare a wall material solution; S2. The pH of the wall material solution is adjusted to 5-6, vitamin B1 and a small molecule emulsifier are added, and then high-speed shearing is performed to fully emulsify the solution; S3. Then spray drying is performed to obtain microcapsule powder.

6. The method for preparing the highly stable vitamin B1 microcapsule powder for soft capsules according to claim 5, characterized in that: The dissolving temperature in step S1 is 65-85°C.

7. The method for preparing the highly stable vitamin B1 microcapsule powder for soft capsules according to claim 5, characterized in that: The shear rate in step S2 is 6000-10000 r / min, and the shear time is 5-10 min.

8. The method for preparing the highly stable vitamin B1 microcapsule powder for soft capsules according to claim 5, characterized in that: The spray drying parameters are: The inlet air temperature is 160~180℃ and the outlet air temperature is 90~100℃.

9. The method for preparing the highly stable vitamin B1 microcapsule powder for soft capsules according to claim 8, characterized in that: The frequency of the atomizer is 300-360 Hz.

10. The method for preparing the highly stable vitamin B1 microcapsule powder for soft capsules according to claim 5, characterized in that: After drying in step S3, the product may be sieved through a 80-120 mesh sieve.

Images