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CN112999206B - Fat-soluble vitamin composition and preparation method thereof - Google Patents

Fat-soluble vitamin composition and preparation method thereof Download PDF

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CN112999206B
CN112999206B CN202110265577.5A CN202110265577A CN112999206B CN 112999206 B CN112999206 B CN 112999206B CN 202110265577 A CN202110265577 A CN 202110265577A CN 112999206 B CN112999206 B CN 112999206B
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fat
vitamin
soluble
soluble vitamin
emulsion
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CN112999206A (en
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徐茂保
江晨
张现涛
何盛江
谭斌
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Guangzhou Baimei Medical Technology Co ltd
Guangzhou Egg Biotechnology Co ltd
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Guangzhou Baimei Medical Technology Co ltd
Guangzhou Egg Biotechnology Co ltd
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Abstract

The application belongs to the technical field of vitamins, and particularly relates to a fat-soluble vitamin composition and a preparation method thereof. The fat-soluble vitamin composition provided by the application comprises the following components in parts by mass: 0.05-5 parts of fat-soluble vitamin; 5-80 parts of an oil phase; 5-50 parts of an emulsifier; 0.1-10 parts of antioxidant; 5-60 parts of auxiliary emulsion; wherein the emulsifier is colloidal silica. The application also provides a preparation method, which comprises the following steps: mixing fat-soluble vitamins and an oil phase to prepare a first mixture; mixing the antioxidant, the co-emulsion, the emulsifier and water to obtain a second mixture; the first mixture and the second mixture are mixed, then dried and sieved to obtain the composition of the fat-soluble vitamins. The fat-soluble vitamin composition and the preparation method thereof can effectively solve the technical problems of low uniformity and easy oxidation and degradation of the existing composite fat-soluble vitamin product.

Description

Fat-soluble vitamin composition and preparation method thereof
Technical Field
The application belongs to the technical field of vitamins, and particularly relates to a fat-soluble vitamin composition and a preparation method thereof.
Background
Vitamins, also known as vitamins (vitamin), are a class of trace organic substances that human and animals must obtain from food in order to maintain normal physiological functions, and play an important role in the growth, metabolism, and development processes of the human body. Vitamins are not constituents constituting tissues and cells of the body, and do not produce energy, and their role is mainly involved in the regulation of the metabolism of the body. Most vitamins, which are not synthesized or synthesized in insufficient amounts by the body, cannot meet the needs of the body and must be obtained from food. The causes of vitamin deficiency are mainly the following 4 cases: 1. food supply is seriously insufficient, and ingestion is insufficient; such as: single food, improper storage, cooking damage, etc. Such as heat loss of folic acid. 2. The absorption and utilization are reduced; such as: digestive system diseases or too little fat intake affect the absorption of fat-soluble vitamins. 3. The vitamin requirement is relatively increased; such as: pregnant and lactation women, children, special work and people in special environment. 4. Improper use of antibiotics can result in increased vitamin requirements.
The human body has small demand for vitamins, and daily demand is usually calculated as milligram (mg) or microgram (microgram), but once lacking, the corresponding vitamin deficiency is caused, which causes damage to human health. Vitamins are classified into fat-soluble vitamins and water-soluble vitamins. Fat-soluble vitamins refer to vitamins which are soluble in fat but insoluble in water and can be stored in the body after being absorbed, and include vitamin A, vitamin D, vitamin E and vitamin K. The vitamin is difficult to mix because the amount of the added vitamin is very small in the process of preparing the medicine. On the other hand, the administration effect is not as expected because vitamins are easily oxidized or degraded.
Disclosure of Invention
In view of this, the present application provides a fat-soluble vitamin composition and a preparation method thereof, which can effectively solve the technical problems of low uniformity, easy oxidation and degradation in the existing composite fat-soluble vitamin product.
In a first aspect, the present application provides a fat-soluble vitamin composition, comprising, in parts by mass:
Figure BDA0002972257210000021
wherein the emulsifier is colloidal silica.
In another embodiment, the method comprises the following steps of:
Figure BDA0002972257210000022
wherein the emulsifier is colloidal silica.
In another embodiment, the method comprises the following steps of:
Figure BDA0002972257210000023
wherein the emulsifier is colloidal silica.
In another embodiment, the fat soluble vitamin is selected from one or more of vitamin a, vitamin D, vitamin E and vitamin K.
In another embodiment, the oil phase is selected from one or more of soybean oil, hydrogenated vegetable oil, petrolatum, liquid paraffin, silicone oil, cholesterol, cetyl alcohol, glycerol monostearate and medium chain triglycerides.
In another embodiment, the antioxidant is selected from one or more of sodium bisulfite, sodium sulfite, sodium thiosulfate, vitamin C, sodium ascorbate, D-isoascorbic acid, vitamin E, tocopherol, thioacetic acid, methionine, lysine, arginine, fumaric acid, maleic acid, disodium edetate, and calcium sodium edetate.
In another embodiment, the co-emulsion is selected from one or more of n-butanol, ethylene glycol, propylene glycol, glycerin, corn starch, pregelatinized starch, and sucrose.
In another embodiment, the fat-soluble vitamin composition is in the form of a tablet, capsule, granule, pill, powder, oral suspension, oral emulsion, powder, or premix.
In another embodiment, the fat-soluble vitamin composition is in the form of an emulsion prepared by a process comprising: adding fat-soluble vitamins and emulsifier into oil phase, dissolving, adding antioxidant and auxiliary emulsion into water, mixing the two solutions, and preparing emulsion with colloid mill, emulsifying machine or homogenizer.
In another embodiment, the fat-soluble vitamin composition is in the form of an emulsion prepared by a process comprising: adding fat-soluble vitamins, antioxidant and auxiliary emulsion into oil phase, dissolving, adding emulsifier into water, mixing the two, and preparing emulsion with colloid mill, emulsifying machine or homogenizer.
In another embodiment, the fat-soluble vitamin composition is in the form of an emulsion prepared by a process comprising: adding fat-soluble vitamins into oil phase, dissolving, adding emulsifier, antioxidant and auxiliary emulsion into water, mixing the two, and preparing emulsion with colloid mill, emulsifying machine or homogenizer.
In a second aspect, the present application provides a process for preparing the fat-soluble vitamin composition, comprising:
step 1, mixing fat-soluble vitamins and an oil phase to prepare a first mixture;
mixing the antioxidant, the co-emulsion, the emulsifier and water to obtain a second mixture;
and 2, mixing the first mixture and the second mixture, and then drying and sieving to obtain the fat-soluble vitamin composition.
In another embodiment, the drying is vacuum freeze drying or spray drying.
Preferably, the drying is vacuum freeze drying.
In another embodiment, step 2 specifically includes: homogenizing the first mixture and the second mixture with a homogenizer at 12000rpm for 10min, drying, and sieving to obtain the composition of fat-soluble vitamins.
In another embodiment, step 2 specifically includes: mixing the first mixture and the second mixture, freeze-drying the mixture in a vacuum freeze dryer, controlling the water content of the dried powder within 1%, and sieving the powder with a 80-mesh sieve to obtain the fat-soluble vitamin composition.
The third aspect of the application provides an application of the composition of the fat-soluble vitamins in preparation of medicines, health products, foods and feeds.
The fat-soluble vitamin composition of the present application is very stable under high temperature and high humidity (60 ℃ C., 75% RH). From the experimental data of the present application it can be seen that:
(1) the fat-soluble vitamin composition has very uniform content distribution and very good fluidity.
(2) The content of the fat-soluble vitamin composition is very close to the theoretical amount, the quality is stable, and the attenuation speed is obviously reduced.
(3) In the production process of the pharmaceutical preparation, the fat-soluble vitamin composition has good oil absorption performance and fluidity due to the addition of a large amount of colloidal silicon dioxide, and can well solve the problems of greasiness and uniform mixing of powder.
(4) In the production process of the pharmaceutical preparation, the fat-soluble vitamin composition is added with a large amount of colloidal silicon dioxide, fat-soluble vitamins and other auxiliary materials, so that the fat-soluble vitamins and the other auxiliary materials are absorbed in tiny pores of the silicon dioxide, and other water-soluble substances (auxiliary emulsion or antioxidant) wrap the fat-soluble vitamin composition, so that the problem of rapid reduction of the content can be well solved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a first angle micrograph of an emulsion provided in example 1 of the present application;
FIG. 2 is a second angle micrograph of an emulsion provided in example 1 of the present application;
fig. 3 is a micrograph of a fat soluble vitamin composition provided in example 1 of the present application;
fig. 4 is a micrograph of a fat soluble vitamin composition provided in example 1 of the present application after reconstitution.
Detailed Description
The application provides a fat-soluble vitamin composition and a preparation method thereof, which are used for solving the technical defects of low uniformity and easy oxidation and degradation in the existing composite fat-soluble vitamin product.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without making any creative effort belong to the protection scope of the present application.
The raw materials and reagents used in the following examples are commercially available or self-made.
Example 1
The present application provides three fat soluble vitamin compositions, methods comprising:
under the condition of keeping out of the sun, according to the mass fractions of the components in table 1, firstly adding vitamin A into medium-chain triglyceride for dissolving, adding sodium ascorbate, sucrose and colloidal silicon dioxide into a proper amount of water, stirring and dispersing, then pouring the two together, homogenizing by using a homogenizer at the rotating speed of 12000rpm for 10min to prepare emulsion, finally carrying out vacuum freeze drying on the emulsion, and passing the dried emulsion through a 80-mesh screen to respectively prepare a sample 1 and a sample 2, namely a sample 3.
TABLE 1
Figure BDA0002972257210000051
As a result of examining micrographs of the emulsion not subjected to vacuum freeze-drying of sample 1 of the present application, as shown in fig. 1 to 2, from fig. 1 to 2, the emulsion not subjected to vacuum freeze-drying produced by the present application had a large amount of medium-chain triglycerides containing fat-soluble vitamins (vitamin a) uniformly distributed therein, and the particle size of the medium-chain triglycerides containing fat-soluble vitamins (vitamin a) reached the micrometer level.
The micrographs of sample 1 (fat-soluble vitamin composition) prepared in the examples of the present application were examined, and as shown in FIG. 3, the fat-soluble vitamin was absorbed into the fine pores of colloidal silica.
As shown in fig. 4, the micrographs of the sample 1 (fat-soluble vitamin composition) prepared in the example of the present application after being redissolved show that the fat-soluble vitamin composition of the present application can be uniformly dispersed in the solution after being redissolved.
Example 2
The present application provides three fat-soluble vitamin compositions, a method comprising:
under the condition of keeping out of the sun, according to the mass fractions of the components in table 2, firstly adding vitamin D3 into medium-chain triglyceride for dissolving, adding sodium ascorbate, sucrose and colloidal silicon dioxide into a proper amount of water, stirring and dispersing, then pouring the two together, homogenizing by using a homogenizer at the rotating speed of 12000rpm for 10min, finally carrying out vacuum freeze drying on the emulsion, and passing the dried emulsion through a 80-mesh screen to respectively prepare a sample 4 and a sample 5, namely a sample 6.
TABLE 2
Figure BDA0002972257210000061
Example 3
The present application provides three fat-soluble vitamin compositions, a method comprising:
under the condition of keeping out of the sun, according to the mass fractions of the components in table 3, firstly adding vitamin E into medium-chain triglyceride for dissolving, adding sodium ascorbate, sucrose and colloidal silicon dioxide into a proper amount of water, stirring and dispersing, then pouring the two together, homogenizing by using a homogenizer at the rotating speed of 12000rpm for 10min, finally carrying out vacuum freeze drying on the emulsion, and passing the dried emulsion through a 80-mesh screen to respectively prepare a sample 7 and a sample 8, namely a sample 9.
TABLE 3
Figure BDA0002972257210000062
Comparative example 1
The present application provides three control products, a method comprising:
under the condition of keeping out of the sun, according to the mass fractions of the components in table 4, firstly adding fat-soluble vitamins into medium-chain triglyceride for dissolving, adding sodium ascorbate, sucrose and colloidal silicon dioxide into a proper amount of water, stirring and dispersing, then pouring the two together, homogenizing by using a homogenizer at the rotating speed of 12000rpm for 10min, finally spray-drying the emulsion, and screening by using a 80-mesh screen after drying to respectively prepare a sample 10 and a sample 11, namely a sample 12.
TABLE 4
Figure BDA0002972257210000071
In Table 4, "NA" is no addition.
Comparative example 2
The present application provides three control products, methods comprising:
under the dark condition, according to the mass fractions of the components in table 5, firstly adding fat-soluble vitamins into medium-chain triglyceride for dissolving, adding sodium ascorbate, sucrose and sodium dodecyl sulfate into a proper amount of water, stirring and dispersing, then pouring the two together, homogenizing by using a homogenizer at the rotating speed of 12000rpm for 10min, finally carrying out vacuum freeze drying on the emulsion, and passing the dried emulsion through a 80-mesh screen to respectively prepare a sample 13 and a sample 14, namely a sample 15.
TABLE 5
Figure BDA0002972257210000072
Figure BDA0002972257210000081
In Table 5, "NA" is no addition.
Comparative example 3
The present application provides three control products, methods comprising:
under the condition of keeping away from light, according to the mass fractions of the components in the table 6, firstly adding fat-soluble vitamins and soybean phospholipids into medium-chain triglyceride for dissolving, adding sodium ascorbate and sucrose into a proper amount of water, stirring and dispersing, then pouring the sodium ascorbate and the sucrose together, homogenizing by using a homogenizer at the rotation speed of 12000rpm for 10min, finally carrying out vacuum freeze drying on the emulsion, and screening the dried emulsion through an 80-mesh screen to respectively prepare a sample 16 and a sample 17, namely a sample 18.
TABLE 6
Figure BDA0002972257210000082
In Table 6, "NA" is no addition.
Example 7
The embodiment of the application provides content determination tests of vitamin A in samples 1-3, 10, 13 and 16, and the method comprises the following steps:
samples 1 to 3, 10, 13 and 16 containing vitamin A, and commercially available vitamin A concentrated powder are respectively sealed by a High Density Polyethylene (HDPE) bottle, and then placed under the conditions of 60 ℃ and 75% RH humidity, and then sampled and detected for relative content at 0 day, 3 months, 6 months and 9 months, wherein the angle of repose is detected at 0 day, and the detection results are shown in Table 7. Wherein, the commercially available vitamin A in Table 7 is pure vitamin A; the commercially available vitamin A concentrated powder is prepared by mixing and drying vitamin A, gelatin, soybean oil, dibutyl hydroxy toluene and sucrose.
TABLE 7
Figure BDA0002972257210000091
Example 8
The embodiment of the application provides content determination tests of vitamin D3 in samples 4-6, sample 11, sample 14 and sample 17, and the method comprises the following steps:
samples 1 to 3, sample 11, sample 14 and sample 17 containing vitamin D3, and a commercially available vitamin D3 and a commercially available vitamin D3 concentrated powder were sealed with high density polyethylene bottles (HDPE), and placed at 60 ℃ and 75% RH, and then sampled at 0 day, 3 months, 6 months and 9 months, respectively, to detect the relative contents, wherein the angle of repose was detected at 0 day, and the detection results are shown in table 8. Among them, commercially available vitamin D3 in table 8 is pure vitamin D3; the commercially available vitamin D3 concentrated powder is prepared by mixing vitamin D3, corn starch, tocopherol, bovine gelatin hydrolysate and hydrogenated soybean oil, and drying.
TABLE 8
Figure BDA0002972257210000092
Figure BDA0002972257210000101
Example 9
The embodiment of the application provides the content determination tests of vitamin E in samples 7 to 9, 12, 15 and 18, and the method comprises the following steps:
samples 7 to 9, 12, 15 and 18 containing vitamin E, and commercially available vitamin E concentrated powder were sealed with High Density Polyethylene (HDPE) bottles, and placed at 60 ℃ and 75% RH humidity, and then sampled at 0 day, 3 months, 6 months and 9 months respectively to detect the relative content, wherein the angle of repose was detected at 0 day, and the detection results are shown in Table 9. Wherein, commercially available vitamin E in table 9 is pure vitamin E; the commercially available vitamin E concentrated powder is prepared by mixing vitamin E, gelatin, Arabic gum, sucrose and lactalbumin and drying.
TABLE 9
Figure BDA0002972257210000102
Figure BDA0002972257210000111
From the results, it can be seen that the stability of samples 1 to 9 is better than that of samples 10 to 12 and the commercial products, especially better than that of the comparative example using spray drying, because the temperature of spray drying is higher by about 150 ℃, and the moisture of the product is also higher, which affect the stability of the samples. In addition, the stability and fluidity of samples 1 to 9 using colloidal silica as the emulsifier are better than those of samples 13 to 18 using sodium lauryl sulfate and soybean lecithin as the emulsifier, and the reason for this is that colloidal silica has strong oil absorption and lubrication properties in addition to the emulsifying properties, and can better protect the fat-soluble vitamins from degradation and promote the fluidity of the powder to ensure the stability and the uniformity.
As is clear from the data in fig. 1 to 4 and tables 7 to 9:
(1) the fat-soluble vitamin composition has very uniform content distribution and very good fluidity.
(2) The content of the fat-soluble vitamin composition is very close to the theoretical amount, the quality is stable, and the attenuation speed is obviously reduced.
(3) In the production process of the pharmaceutical preparation, the fat-soluble vitamin composition has good oil absorption performance and fluidity due to the addition of a large amount of colloidal silicon dioxide, and can well solve the problems of greasiness and uniform mixing of powder.
(4) In the production process of the pharmaceutical preparation, the fat-soluble vitamin composition is added with a large amount of colloidal silicon dioxide, fat-soluble vitamins and other auxiliary materials, so that the fat-soluble vitamin composition can be absorbed in fine pores of the colloidal silicon dioxide, and other water-soluble substances (auxiliary emulsion or antioxidant) wrap the fat-soluble vitamin composition, so that the problem of rapid reduction of the content can be well solved.
The foregoing is only a preferred embodiment of the present application and it should be noted that those skilled in the art can make several improvements and modifications without departing from the principle of the present application, and these improvements and modifications should also be considered as the protection scope of the present application.

Claims (4)

1. A fat-soluble vitamin composition is characterized by comprising the following components in parts by mass:
Figure FDA0003806720790000011
wherein the emulsifier is colloidal silica;
the auxiliary emulsion is selected from one or more of corn starch, pregelatinized starch and sucrose;
the oil phase is selected from one or more of glyceryl monostearate and medium chain triglycerides;
the preparation method of the fat-soluble vitamin composition comprises the following steps:
step 1, mixing the fat-soluble vitamins and the oil phase to prepare a first mixture;
mixing said antioxidant, said co-emulsion, said emulsifier and water to produce a second mixture
And 2, mixing the first mixture and the second mixture, and then carrying out vacuum freeze drying and sieving to obtain the fat-soluble vitamin composition.
2. The fat-soluble vitamin composition according to claim 1, wherein the fat-soluble vitamin is selected from one or more of vitamin A, vitamin D, vitamin E, and vitamin K.
3. The fat-soluble vitamin composition according to claim 1, wherein the antioxidant is selected from one or more of sodium bisulfite, sodium sulfite, sodium thiosulfate, vitamin C, sodium ascorbate, D-erythorbic acid, vitamin E, thioacetic acid, methionine, lysine, arginine, fumaric acid, maleic acid, edetate disodium, and edetate calcium sodium.
4. The fat-soluble vitamin composition according to any one of claims 1 to 3, wherein the dosage form of the fat-soluble vitamin composition is tablet, capsule, granule, pill, powder, oral suspension, oral emulsion or premix.
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