Preparation method and application of mineral oral liquid containing fat-soluble vitamins

Abstract

The invention provides a preparation method and application of a mineral oral liquid containing fat-soluble vitamins, the fat-soluble vitamins are dissolved in an oil phase, then the oil phase is mixed with a water phase containing an emulsifier, and high-shear and high-pressure homogenization treatment is performed to obtain emulsified fat-soluble vitamins; dispersing the sweetening agent, the suspending aid, the pH regulator and the insoluble mineral substances to obtain a mixed solution; adding the emulsified fat-soluble vitamins and the flavor regulator into the mixed solution, adding water to a constant volume, and uniformly stirring to obtain a material solution; and canning the feed liquid, sealing, and sterilizing at high temperature to obtain the oral liquid. The fat-soluble vitamins in the oral liquid provided by the invention are small in particle size after being subjected to high-shear and high-pressure homogenization treatment, can tolerate high-temperature sterilization, is small in loss rate, good in dispersity and high in stability within the shelf life, and can maintain the actual content of the fat-soluble vitamins in the oral liquid and ensure the nutritional effect of the fat-soluble vitamins.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of food technology, and specifically relates to a preparation method of a mineral oral liquid containing fat-soluble vitamins and application thereof. BACKGROUND

[0002] The mineral oral liquid containing fat-soluble vitamins is a dosage form of a nutritional supplement that is favored at present. It wins the favor of many consumers due to the advantages of high mineral content and smooth taste. Moreover, the addition of fat-soluble vitamins in the oral liquid can form a good synergistic effect with minerals, further improving the nutritional efficacy of the product. However, such products also face some technical problems in the production and storage process. Fat-soluble vitamins are not only sensitive to high temperature, but also prone to structural damage during high-temperature sterilization. Moreover, the stability of fat-soluble vitamins in aqueous solution systems is generally poor, and there is a significant decay during the shelf life, which seriously affects the actual content and nutritional effect of fat-soluble vitamins in the oral liquid product. One of the common methods to improve the stability of fat-soluble vitamins is to prepare microcapsule powder of fat-soluble vitamins, and then disperse it in an aqueous solution system. However, the commonly used microcapsule powders on the market cannot meet the long-term stability requirements, and continuously decay during normal temperature storage. Moreover, due to the characteristics of the embedding wall material, some microcapsule powders are prone to uneven dispersion, sedimentation and other problems in aqueous solutions, which brings certain difficulties to product application. Another method to improve the stability of fat-soluble vitamins is to prepare a self-emulsifying system of fat-soluble vitamins and surfactants. The core of the self-emulsifying system is the balanced system of oil phase, surfactant and co-surfactant. This balance is easily destroyed by external conditions or time, leading to the failure of the system. The self-emulsifying system needs to add a high proportion of surfactants, which may cause local or systemic safety problems: high-concentration surfactants such as Tween 80 can damage the gastrointestinal mucosal barrier, stimulate mucosal cells, and cause symptoms such as nausea, vomiting, diarrhea, and stomach discomfort. The risk of side effects is higher, especially for people with sensitive gastrointestinal tracts.

[0003] CN 117678758 A discloses a composition containing fat-soluble vitamins, which comprises 12-35% of insoluble calcium salt, 0.00002-1.5% of fat-soluble vitamins, 0.5-2.5% of vegetable oil, 0.5-2.5% of emulsifier, and water; its preparation method comprises uniformly mixing fat-soluble vitamins and vegetable oil, heating at 60-85°C to obtain an oil phase, uniformly mixing emulsifier and water to obtain an aqueous phase, adding the oil phase into the aqueous phase, stirring to obtain an emulsion; adding insoluble calcium salt into the emulsion, stirring to obtain the composition. By controlling the particle size of insoluble calcium salt and limiting the mass fraction of fat-soluble vitamins in the composition, the oil-in-water structure formed by fat-soluble vitamins in the composition is more stable, and fat-soluble vitamins are more stable in the liquid preparation. Although the composition provided by the patent has certain stability, the patent only takes 60-85°C treatment when preparing the oil phase, which is difficult to ensure that there is no microbial risk. At the same time, the patent does not verify the long-term stability of the composition, and the stability of the composition during the shelf life cannot be determined. CN 119924531 A discloses a preparation method of ultra-micro emulsified liquid calcium for improving the utilization rate of calcium, VD and VK. The preparation method comprises adding calcium citrate, 0.1-2 parts of suspending agent, 0.1-1 part of acidifying agent, 5-15 parts of sweetening agent, 0.1-2 parts of essence, and 60-90 parts of water into an emulsifying pot and stirring uniformly, adding vitamin D, vitamin K 20-60 parts, and emulsifier 30-50 parts, and auxiliary emulsifier 0-50 parts to form a self-emulsifying system, and then stirring uniformly to obtain a mixture. The mixture is subjected to high-speed shearing treatment at 5000 rpm / min and 35-40 min, and then the initial emulsified liquid is obtained. The initial emulsified liquid is subjected to high-pressure homogenization treatment at 400-800 bar for 1-2 times to obtain the ultra-micro emulsified liquid calcium. The oil-water separation phenomenon occurs after 3500 rpm centrifugation for 10 min in Example 3 and Example 4 of the patent, and the effective content and long-term stability of fat-soluble vitamins are not verified. At the same time, high-temperature sterilization treatment is not carried out, which is difficult to ensure that there is no microbial risk.

[0004] In summary, the fat-soluble vitamins in the mineral oral liquid on the market are usually treated by microcapsule powder and self-emulsifying system, and the average particle size of the obtained fat-soluble vitamins is 5-10 μm. In order to reduce the loss, low-temperature sterilization at <100°C is usually used. Under such conditions, the fat-soluble vitamins are prone to coalescence and delamination, which greatly affects the appearance and taste of the product. Moreover, the stability during the subsequent shelf life is difficult to maintain, and the activity gradually decreases with the extension of storage time, and the nutritional ingredients are continuously lost. At the same time, the sterilization temperature of <100°C is not enough to completely kill all microorganisms, which poses a risk of microbial growth and brings potential safety hazards to the product. SUMMARY

[0005] To solve the technical problems of the above-mentioned mineral oral liquid containing fat-soluble vitamins, such as large particle size of fat-soluble vitamins, easy coalescence, stratification phenomenon affecting product taste and appearance, unable to withstand high temperature sterilization causing fat-soluble vitamins degradation, easy microbial risk, poor shelf stability and easy degradation of nutrients, the present application provides a preparation method of a mineral oral liquid containing fat-soluble vitamins and application thereof.

[0006] To achieve the above-mentioned application purposes, the technical solutions of the present application are as follows: In the first aspect of the present application, the present application provides a preparation method of a mineral oral liquid containing fat-soluble vitamins, comprising the following steps: S1. Dissolving fat-soluble vitamins in a base oil to obtain an oil phase, dissolving an emulsifier in purified water to obtain an aqueous phase, mixing the oil phase and the aqueous phase, and then high-pressure homogenization after high shear to obtain emulsified fat-soluble vitamins; S2. Putting a sweetener, a suspending agent and a pH regulator into water, dissolving completely, and then adding a poorly soluble mineral to disperse to obtain a mixed solution; S3. Adding emulsified fat-soluble vitamins and a flavor regulator to the mixed solution, adding water to constant volume, and stirring uniformly to obtain a feed solution; S4. Canning the feed solution, sealing, sterilizing to obtain the oral liquid; Further, the surface area average diameter D(3,2) of the emulsified fat-soluble vitamins is 100-500 nm, and the volume average diameter D(4,3) is 0.5-3 μm.

[0007] In one embodiment, the surface area average diameter D(3,2) of the emulsified fat-soluble vitamins is 150-450 nm, and the average volume diameter D(4,3) is 0.6-3 μm.

[0008] Preferably, the surface area average diameter D(3,2) of the emulsified fat-soluble vitamins is 199-431 nm, and the volume average diameter D(4,3) is 0.6-2.6 μm; more preferably, the surface area average diameter D(3,2) of the emulsified fat-soluble vitamins is 199 nm, and the volume average diameter D(4,3) is 0.682 μm.

[0009] In one embodiment, the high shear condition is 6000-15000 rpm for 10-15 min; the high-pressure homogenization pressure is 200-500 bar; and the sterilization condition is 100-125 ℃ for 15-45 min.

[0010] Preferably, the high shear conditions are 10,000 - 15,000 rpm for 12 - 15 min; the high pressure homogenization pressure is 300 - 500 bar; the sterilization temperature is 105 - 121 ℃, and the sterilization time is 30 min.

[0011] In one embodiment, the fat-soluble vitamin includes one or more of vitamin D, vitamin K, vitamin A, and vitamin E.

[0012] In one embodiment, the fat-soluble vitamin accounts for 0.00001% - 0.001% of the mass of the oral liquid, preferably 0.000065% of the mass of the fat-soluble vitamin in the oral liquid.

[0013] In one embodiment, the insoluble mineral includes one or more of the following: calcium citrate, calcium citrate malate, calcium lactate, calcium malate, and / or insoluble salts of minerals such as magnesium, selenium, iron, and zinc.

[0014] In one embodiment, the sparingly soluble minerals account for 5-20% of the mass of the oral liquid, preferably 15% by mass.

[0015] In one embodiment, the base oil includes one or more of soybean oil, rapeseed oil, olive oil, walnut oil, peanut oil, sunflower oil, and corn oil, preferably soybean oil.

[0016] In one embodiment, the base oil accounts for 0.2-1.0% of the mass of the oral liquid, preferably 0.8% of the mass of the base oil in the oral liquid.

[0017] In one embodiment, the emulsifier includes one or more of gum arabic, sodium octenyl succinate starch, sucrose ester, and polyglycerol ester, preferably gum arabic.

[0018] In one embodiment, the emulsifier accounts for 0.1-0.8% of the mass of the oral liquid, preferably 0.4% of the mass of the oral liquid.

[0019] In one embodiment, the sweetener includes one or more of xylitol, sorbitol, erythritol, sucralose, steviol glycosides, and mannitol, preferably xylitol.

[0020] In one embodiment, the sweetener accounts for 0.02-15% of the oral liquid by mass, preferably 10% of the oral liquid by mass.

[0021] In one embodiment, the suspending agent includes one or more of xanthan gum, gellan gum, guar gum, and locust bean gum, preferably xanthan gum.

[0022] In one embodiment, the suspending agent accounts for 0.1-0.8% of the mass of the oral liquid, preferably 0.15% of the mass of the oral liquid.

[0023] In one embodiment, the pH adjuster includes one or more of citric acid, malic acid, lactic acid, tartaric acid, and fumaric acid, preferably citric acid.

[0024] In one embodiment, the pH adjuster accounts for 0.1-1% of the mass of the oral liquid, preferably 0.5% of the mass of the oral liquid.

[0025] In one embodiment, the flavor modifier is one or more of food flavorings, fruit juices, and fruit powders.

[0026] In one embodiment, the flavor modifier accounts for 0.1-1% of the mass of the oral liquid.

[0027] In a second aspect, the present invention provides an oral mineral solution containing fat-soluble vitamins, wherein, by mass percentage, the oral solution comprises 0.00001% - 0.001% fat-soluble vitamins, 5 - 20% insoluble minerals, 0.2 - 1.0% base oil, 0.1 - 0.8% emulsifier, and water.

[0028] In one embodiment, the oral liquid further includes one or more of sweeteners, suspending agents, pH adjusters, and flavor modifiers.

[0029] In one embodiment, the sweetener is 0.02-15% by mass, the suspending agent is 0.1-0.8%, the pH adjuster is 0.1-1%, and the flavor modifier is 0.1-1%.

[0030] Beneficial effects The preparation method and application of the oral mineral solution containing fat-soluble vitamins provided by this invention have the following technical effects: (1) Fat-soluble vitamins have a low loss rate after high-temperature sterilization, and still have a high content in oral liquids without microbial risk; (2) Fat-soluble vitamins have small particle size, good dispersibility in oral liquids, and are not easy to aggregate or disperse, so as not to affect the appearance and taste of the product. (3) Small-particle-size emulsified fat-soluble vitamins treated with high-temperature sterilization, high shear and high-pressure homogenization have high shelf-life stability and are not easily lost. Attached Figure Description

[0031] Figure 1 The particle size distribution diagram of the oral liquid prepared according to this technical solution is shown. Figure 2 This is a particle size distribution diagram of commercially available oral mineral solutions containing fat-soluble vitamins. Figure 3 This is a diagram showing the effect of centrifugation of the oral liquid according to an embodiment of the present invention. Figure 3 In section B, the lines indicate the location of the layered interface. Detailed Implementation

[0032] The embodiments of the present invention will be described in detail below with reference to examples. However, those skilled in the art will understand that the following examples are for illustrative purposes only and should not be considered as limiting the scope of the invention. Unless otherwise specified in the examples, conventional conditions or conditions recommended by the manufacturer are followed. Reagents or instruments whose manufacturers are not specified are all commercially available conventional products.

[0033] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0034] As used herein, the terms “and / or,” “or / and,” and “and / or” may include any one of two or more of the related listed items, as well as any and all combinations of the related listed items, including any two related listed items, any more related listed items, or a combination of all the related listed items.

[0035] In this invention, terms such as "first aspect" and "second aspect" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or quantity, nor should they be construed as implicitly indicating the importance or quantity of the indicated technical features. Moreover, terms such as "first" and "second" serve only as a non-exhaustive enumeration and should be understood not to constitute a closed limitation on the quantity.

[0036] In this invention, the technical features described in an open-ended manner include both closed-ended technical solutions composed of the listed features and open-ended technical solutions that include the listed features.

[0037] In this invention, 0 months refers to the accelerated testing conditions after sample sterilization: 37 ± 2 ℃, RH 75 ± 5%.

[0038] Example 1: This embodiment prepares an oral solution containing fat-soluble vitamins according to the following steps: S1. Dissolve vitamin D3 in soybean oil to obtain the oil phase, dissolve gum arabic in purified water to obtain the aqueous phase, mix the two, and homogenize under high shear at 15000 rpm for 15 min, followed by high pressure homogenization at 500 bar to obtain emulsified vitamin D3.

[0039] S2. Add xylitol, xanthan gum, and citric acid to water, and after they are completely dissolved, add calcium citrate to disperse them, thus obtaining a mixed solution.

[0040] S3. Add emulsified vitamin D3 and edible flavoring to the mixture, add water to make up to the target volume, stir well to obtain the liquid.

[0041] S4. Fill and seal the liquid, then place it in an autoclave and sterilize at 105 ℃ for 30 min.

[0042] The proportions of each material used in this embodiment are as follows: Vitamin D3 0.000065%, soybean oil 0.8%, gum arabic 0.4%, xylitol 10%, xanthan gum 0.15%, citric acid 0.5%, and calcium citrate 15%.

[0043] Example 2: The preparation method in this embodiment is the same as in Example 1, except that the sterilization temperature is 115 ℃.

[0044] Example 3: The preparation method in this embodiment is the same as in Example 1, except that the sterilization temperature is 121 °C.

[0045] Example 4: The preparation method in this embodiment is the same as in Example 1. The only difference between this embodiment and Example 1 is that the shearing speed is 6000 rpm, the shearing time is 10 min, and the high-pressure homogenization pressure is 200 bar.

[0046] Example 5: The preparation method in this embodiment is the same as in Example 1. The only difference between this embodiment and Example 1 is that the shearing speed is 6000 rpm, the shearing time is 10 min, the high-pressure homogenization pressure is 200 bar, and the sterilization temperature is 115 ℃.

[0047] Example 6 The preparation method in this embodiment is the same as in Example 1. The only difference between this embodiment and Example 1 is that the shearing speed is 6000 rpm, the shearing time is 10 min, the high-pressure homogenization pressure is 200 bar, and the sterilization temperature is 121 ℃.

[0048] Example 7: The preparation method in this embodiment is the same as in Example 1. The only difference from Example 1 is that the shearing speed is 12000 rpm, the shearing time is 12 min, the high-pressure homogenization pressure is 400 bar, and the fat-soluble vitamins include VD3 and VK.

[0049] Example 8: The preparation method in this embodiment is the same as in Example 1. The only difference between this embodiment and Example 1 is that the shearing speed is 10,000 rpm, the shearing time is 12 min, and the high-pressure homogenization pressure is 300 bar.

[0050] Example 9: The preparation method in this embodiment is the same as in Example 1, except that the fat-soluble vitamins include VD3 and VK.

[0051] Example 10: The preparation method in this embodiment is the same as in Example 1. The only difference between this embodiment and Example 1 is that the shearing speed is 10,000 rpm, the shearing time is 12 min, the high-pressure homogenization pressure is 300 bar, and the insoluble calcium salt is calcium citrate malate.

[0052] Example 11: The preparation method of this embodiment is the same as that of Example 1. The only difference between this embodiment and Example 1 is that the suspending agent is gellan gum and the pH adjuster is lactic acid.

[0053] Comparative Example 1: The preparation method of this comparative example is the same as that of Example 1, except that the high-pressure homogenization pressure is 150 bar.

[0054] Comparative Example 2: The preparation method of this comparative example is the same as that of Example 8, except that the high-pressure homogenization pressure is 600 bar.

[0055] Comparative Example 3: The preparation method of this comparative example is the same as that of Example 8, except that the shearing speed is 5000 rpm and the shearing time is 5 min.

[0056] Comparative Example 4: The preparation method of this comparative example is based on Example 1 of CN 117678758 A. The difference between this example and Example 1 of the present invention is that the shearing speed is 10000 rpm, the shearing time is 5 min, and there is no high-pressure homogenization step.

[0057] Comparative Example 5: The preparation method of this comparative example is based on Example 1 of CN 117678758 A. The difference between this example and Example 1 of the present invention is that the shearing speed is 10000 rpm, the shearing time is 5 min, the sterilization temperature is 85 ℃, and there is no high-pressure homogenization step.

[0058] Comparative Example 6: The preparation method of this comparative example is based on Example 1 of CN 119924531 A. The only difference between this example and Example 7 of the present invention is that the shearing speed is 5000 rpm, the shearing time is 40 min, and the high-pressure homogenization treatment at 400 bar is performed twice.

[0059] Comparative Example 7: The preparation method of this comparative example is based on Example 2 of CN 119924531 A. The only difference between this example and Example 9 of the present invention is that the shearing speed is 5000 rpm, the shearing time is 40 min, and the high-pressure homogenization treatment at 500 bar is performed twice.

[0060] Comparative Example 8: The preparation method of this comparative example is based on Example 3 of CN 119924531 A. The only difference between this example and Example 7 of the present invention is that the shearing speed is 5000 rpm, the shearing time is 35 min, and the high-pressure homogenization treatment at 600 bar is performed twice.

[0061] Comparative Example 9: The preparation method of this comparative example is based on Example 4 of CN 119924531 A. The only difference between this example and Example 7 of the present invention is that the shearing speed is 5000 rpm, the shearing time is 35 min, and the high-pressure homogenization treatment at 800 bar is performed twice.

[0062] Comparative Example 10: This comparative example uses microcapsule powder to prepare a mineral oral liquid containing fat-soluble vitamins. The difference between this example and Example 1 is that it does not include the high-shear, high-pressure homogenization process.

[0063] I. Loss rate of fat-soluble vitamins before and after sterilization The sterilization loss rate of fat-soluble vitamins = 100% - (fat-soluble vitamin content after sterilization / fat-soluble vitamin content before sterilization)%. Referring to Table 1, the loss rate of fat-soluble vitamins in Examples 1-11 did not exceed 8%, with the loss rate of fat-soluble vitamins in Example 8 being only 4.00%. In contrast, the loss rates of fat-soluble vitamins in Comparative Examples 1-3 were all higher than 20%, a difference of 3-5 times. This indicates that when the high-pressure homogenization pressure is too high or too low, or the high shear rate and time are insufficient, fat-soluble vitamins cannot withstand high-temperature sterilization, resulting in significant losses. However, the vitamin and mineral oral liquid prepared by the method of this invention exhibits high stability and low loss rate of fat-soluble vitamins.

[0064] Referring to Example 1 of CN 117678758 A (high shear only, no high pressure homogenization), the loss rates of fat-soluble vitamins in Comparative Example 4 (sterilization temperature 105 ℃) and Comparative Example 5 (sterilization temperature 85 ℃) were 25.54% and 8.15%, respectively, with a significant difference of 17.39%. This indicates that the fat-soluble vitamin and mineral oral solution prepared by CN 117678758 A cannot withstand high-temperature sterilization above 100 ℃, posing a risk of microbial growth. In contrast, the loss rates of Examples 1-11 prepared according to the method of this invention differed by a maximum of only 3.85%, indicating that the fat-soluble vitamins in the vitamin and mineral oral solution prepared by the method of this invention can withstand high-temperature sterilization above 100 ℃, maintaining the content of fat-soluble vitamins while reducing the risk of microbial growth.

[0065] According to CN 119924531A, Examples 1-2 (shear conditions: 5000 rpm for 40 min, high-pressure homogenization pressures: 400 bar and 500 bar), the loss rates of fat-soluble vitamins in Comparative Examples 6-7 were 24.31% and 24.62%, respectively. These rates are nearly 6 times higher than those in Examples 7 and 9 under the same homogenization pressure, indicating that even with high-pressure homogenization, slow high-shear rates are not conducive to the stability of fat-soluble vitamins. Similarly, according to CN 119924531A, Examples 3-4 (shear conditions: 5000 rpm for 35 min, high-pressure homogenization pressures: 600 bar and 800 bar), the loss rates of fat-soluble vitamins in Comparative Examples 8-9 were 26.00% and 28.92%, respectively. These rates are approximately 4 times higher than those in Examples 1-11. The 7-fold increase indicates that when the high shear rate is slow and the high pressure homogenization pressure is too high, it can also lead to the degradation of fat-soluble vitamins, which is detrimental to their stability.

[0066] The loss rate of fat-soluble vitamins in Comparative Example 10 (prepared using microcapsule powder) was 16.96%, which was 2-4 times lower than that in Examples 1-11. This indicates that the preparation method of the present invention is more conducive to the stability of fat-soluble vitamins in vitamin and mineral oral liquids and can maintain the effective content compared with the common microcapsule powder treatment method.

[0067] Table 1. Loss rate of fat-soluble vitamins under different treatment conditions

[0068] II. Dispersion Reference Figure 1 , Figure 2 , Figure 1 In the oral liquid prepared according to the technical solution of this invention, the peaks of fat-soluble vitamins and insoluble calcium salts do not overlap. The particle size distribution of fat-soluble vitamins is in a smaller range, while the particle size distribution of insoluble calcium salts is in a larger range. The fat-soluble vitamins and calcium salt particles of this invention are more likely to form an encapsulated structure, making them more stable to temperature changes and easier to disperse. Figure 2 In commercially available oral liquids, the peaks of soluble vitamins and insoluble calcium salts overlap, and their particle sizes are distributed at around 5 μm, significantly larger than the particle size of the fat-soluble vitamins in this invention. This means that the fat-soluble vitamins and insoluble calcium salts in commercially available oral liquids have similar particle sizes, making it difficult to form the outer coating structure of this invention. This also makes commercially available oral liquids more sensitive to changes in external temperature, more prone to agglomeration into large particles, and difficult to disperse, resulting in stratification. The oral liquid prepared according to the technical solution of this invention has smaller fat-soluble vitamin particle sizes, which is more conducive to the stability of fat-soluble vitamins in mineral oral liquids and improves their dispersibility.

[0069] Reference Figure 3 The dispersibility of fat-soluble vitamins was evaluated by observing the separation after centrifugation at 4000 rpm for 5 min. No separation was observed in Examples 1-11, while separation was observed in Comparative Examples 1-4 and 6-10. This indicates that the fat-soluble vitamins prepared by the method of this invention have good dispersibility in mineral oral solutions and are not prone to aggregation or separation.

[0070] III. Stability Examples 12-14 were prepared using the same method as in Example 8. The only difference between Examples 12-14 and Example 8 is that the fat-soluble vitamins in Examples 12-14 are vitamin A, vitamin E, and vitamin K, respectively.

[0071] The accelerated loss rate of fat-soluble vitamins = loss rate after 3 months of acceleration - loss rate after 0 months, where the loss rate after 0 months is the sterilization loss rate in Table 1. The loss rate for each month during the accelerated testing period = 100% - (fat-soluble vitamin content in the month of testing / fat-soluble vitamin content before sterilization)%. Referring to Table 2, the loss rate of fat-soluble vitamins after 3 months of acceleration in Examples 1-11 did not exceed 11%, with the loss rate of fat-soluble vitamins in Example 8 being only 7.47%, while the loss rates of fat-soluble vitamins in Comparative Examples 1-3 were all higher than 20%, a difference of nearly 3 times. This indicates that the long-term stability and low loss rate of fat-soluble vitamins in the vitamin and mineral oral liquid prepared by the method of this invention are high.

[0072] According to CN 117678758 A, the loss rate of fat-soluble vitamins in Comparative Example 4 prepared by Example 1 was 20.98%, while the loss rate of Examples 1-11 prepared according to the preparation method of the present invention was the highest at 10.85%, which is 2 times higher. This indicates that the small-particle-size emulsified fat-soluble vitamins obtained by high-pressure homogenization of the present invention have high stability during the shelf life.

[0073] According to CN 119924531 A, the loss rates of fat-soluble vitamins in Comparative Examples 6 and 7 prepared in Examples 1-2 after 3 months of accelerated homogenization were 17.75% and 22.07%, respectively. These rates differed by approximately two times from the loss rates in Examples 7 and 9 under the same homogenization pressure. This indicates that even with high-pressure homogenization, a slow high shear rate is not conducive to the long-term stability of fat-soluble vitamins. Similarly, the loss rates of fat-soluble vitamins in Comparative Examples 8 and 9 prepared in Examples 3-4 of CN 119924531 A were 22.22% and 20.40%, respectively. These rates differed by approximately two times from those in Examples 1-11. This suggests that a slow high shear rate and excessively high high-pressure homogenization pressure can also lead to the degradation of fat-soluble vitamins, which is detrimental to their long-term stability.

[0074] The loss rate of fat-soluble vitamins in Comparative Example 10 after 3 months of accelerated processing was 25.10%, which was significantly higher than the loss rate of fat-soluble vitamins in Examples 1-11 of this invention after 3 months of accelerated processing. The difference between the two was 2-3 times, indicating that the small-particle-size emulsified fat-soluble vitamins obtained by high-pressure homogenization of this invention have high stability during the shelf life.

[0075] Referring to Table 3, the loss rates of Examples 12-14 after three months of accelerated processing were 4.84%, 3.91%, and 4.75%, respectively, significantly lower than the loss rates in Comparative Examples 1-10. This indicates that the preparation method of the present invention is applicable to various common fat-soluble vitamins and has a wide range of applications.

[0076] Table 2. Loss of fat-soluble vitamins after acceleration

[0077] Table 3. Accelerated loss rate of other fat-soluble vitamins over three months

[0078] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A method for preparing a mineral oral solution containing fat-soluble vitamins, characterized by, Comprising the following steps: S1. Dissolve the fat-soluble vitamin in the base oil to obtain an oil phase, dissolve the emulsifier in purified water to obtain an aqueous phase, mix the oil phase and the aqueous phase, and then high-pressure homogenization after high shear to obtain emulsified fat-soluble vitamin; S2. Put the sweetener, suspending agent, and pH regulator into water, dissolve completely, and then add the poorly soluble mineral to disperse to obtain a mixed solution; S3. Add the emulsified fat-soluble vitamin and flavor regulator to the mixed solution, add water to constant volume, and stir uniformly to obtain a feed solution; S4. Package, seal, and sterilize the feed solution to obtain the oral solution.

2. Further, the surface area average diameter D(3,2) of the emulsified fat-soluble vitamin is 100-500 nm, and the volume average diameter D(4,3) is 0.5-3 μm.

3. The production method according to claim 1, wherein The high shear condition is 6000-15000 rpm for 10-15 min, and the high-pressure homogenization pressure is 200-500 bar; the sterilization condition is 100-125 ℃ for 15-45 min.

4. The production method according to claim 1, wherein The surface area average diameter D(3,2) of the emulsified fat-soluble vitamin is 150-450 nm, and the average volume diameter D(4,3) of the emulsified fat-soluble vitamin is 0.6-3 μm; preferably, the surface area average diameter D(3,2) of the emulsified fat-soluble vitamin is 199-431 nm; and the average volume diameter D(4,3) of the emulsified fat-soluble vitamin is 0.6-2.6 μm.

5. The production method according to claim 1, wherein The mass ratio of the fat-soluble vitamin is 0.00001 %-0.001 %, and the fat-soluble vitamin includes one or more of vitamin D, vitamin K, vitamin A, and vitamin E.

6. The production method according to claim 1, wherein The mass ratio of the poorly soluble mineral is 5-20 %, and the poorly soluble mineral includes one or more of the poorly soluble salts of calcium citrate, calcium citrate malate, calcium lactate, calcium malate and / or magnesium, selenium, iron, zinc, and other minerals.

7. The production method according to claim 1, wherein Further comprising one or more of the following features: (1) The mass ratio of the base oil is 0.2-1.0 %, and the base oil includes one or more of soybean oil, rapeseed oil, olive oil, walnut oil, peanut oil, sunflower oil, and corn oil; (2) The mass ratio of the emulsifier is 0.1-0.8 %, and the emulsifier includes one or more of gum arabic, sodium octenyl succinate starch, sucrose ester, and polyglycerol ester; (3) The mass ratio of the sweetener is 0.02-15 %, and the sweetener includes one or more of xylitol, sorbitol, erythritol, sucralose, steviol glycoside, and mannitol; (4) The mass ratio of the suspending agent is 0.1-0.8 %, and the suspending agent includes one or more of xanthan gum, gellan gum, guar gum, and locust bean gum; (5) The mass ratio of the pH regulator is 0.1-1 %, and the pH regulator includes one or more of citric acid, malic acid, lactic acid, tartaric acid, and fumaric acid; (6) The mass ratio of the flavor modifier is 0.1-1%, and the flavor modifier is one or more of food essence, fruit juice, and fruit powder.

8. A mineral oral solution containing fat-soluble vitamins prepared by the method according to any one of claims 1 to 7, characterized in that, The mass ratio of the fat-soluble vitamin is 0.00001-0.001%, the mass ratio of the poorly soluble mineral is 5-20%, the mass ratio of the base oil is 0.2-1.0%, the mass ratio of the emulsifier is 0.1-0.8%, and the mass ratio of the water is 70-90%.

9. The oral solution of claim 8, wherein, The oral liquid further comprises one or more of a sweetening agent, a suspending agent, a pH modifier, and a flavor modifier.

10. The oral solution of claim 9, wherein, The mass ratio of the sweetening agent is 0.02-15%, the mass ratio of the suspending agent is 0.1-0.8%, the mass ratio of the pH modifier is 0.1-1%, and the mass ratio of the flavor modifier is 0.1-1%.

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