Solid fat vitamin C microcapsule and preparation method thereof

Abstract

The invention discloses a solid fat vitamin C microcapsule and a preparation method thereof, and belongs to the technical field of vitamin C microcapsule preparation. Vitamin C is wrapped in a hydrophobic wall material, so that water vapor and oxygen can be effectively isolated, and the product stability is improved. The preparation method has the advantages that the preparation process is simple, the release control effect is achieved, loss caused by leakage in the processing step can be reduced, a mixture of active substances and molten lipid materials is atomized in a cold chamber in a spray condensation mode, the high-temperature preparation environment is avoided, and the heat-sensitive vitamin C is well protected; liquid oil with an unsaturated structure is added into solid lipid, and combination of liquid lipid and solid lipid leads to ordered disorder of a large number of crystals. The obtained lipid particle matrix shows great defects on crystal lattices and leaves enough space for accommodating medicine molecules, so that the medicine carrying capacity of the medicine is improved, and the encapsulation efficiency is effectively improved.

Description

Technical Field

[0001] The invention belongs to the technical field of vitamin C microcapsule preparation, and specifically relates to a solid fat vitamin C microcapsule and a preparation method thereof. Background Art

[0002] As a highly effective antioxidant, vitamin C can remove melanin deposits on the skin caused by the acquired environment. It also has the function of scavenging active free radicals and has good whitening, anti-wrinkle and antioxidant effects. Due to its low price, vitamin C has become a nutritional enhancer favored by many food manufacturers. However, vitamin C has strong reducing properties and high water solubility, and is easily affected by external conditions, such as high concentrations of oxygen, high temperatures, alkaline environments, metal ions, ultraviolet rays, etc. In particular, its aqueous solution is more susceptible to oxidation and decomposition, so microencapsulation technology is usually used to stabilize vitamin C.

[0003] Currently, most vitamin C microcapsules use water-soluble wall materials, which are very easy to dissolve and leak in water, and have limited protection for vitamin C during processing. In addition, common processing methods such as spray drying require evaporation of water at high temperatures (140-160°C), which can easily damage vitamin C. Therefore, a method suitable for heat-sensitive substances and controlled release is urgently needed to overcome the problem of inefficient use of vitamin C during processing steps and product storage. 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 solid lipid vitamin C microcapsule.

[0007] In order to solve the above technical problems, the present invention provides the following technical solutions: comprising:

[0008] Using crushed and sieved vitamin C powder as the core material;

[0009] A molten wall material liquid obtained by melting solid fat, liquid oil and emulsifier is used as the wall material;

[0010] The solid fat vitamin C microcapsule is obtained by wrapping the core material with the wall material, wherein the mass ratio of the core material to the wall material is 6:4 to 2:8.

[0011] As a preferred embodiment of the solid fat vitamin C microcapsules of the present invention, the vitamin C powder is sieved through a mesh number of 90 to 130.

[0012] As a preferred embodiment of the solid fat vitamin C microcapsule of the present invention, the solid fat comprises one of hydrogenated palm oil, hydrogenated rapeseed oil, stearic acid and lauric acid;

[0013] The liquid oil includes one of soybean oil, peanut oil, corn oil, and oleic acid;

[0014] The emulsifier includes one of phospholipids and polyglycerol ricinoleate.

[0015] As a preferred embodiment of the solid fat vitamin C microcapsules of the present invention, the mass ratio of the solid fat to the liquid oil is 6:4 to 10:0.

[0016] As a preferred embodiment of the solid fat vitamin C microcapsules of the present invention, the amount of the emulsifier is 0-2% of the total mass of the solid fat and the liquid oil.

[0017] As a preferred embodiment of the solid fat vitamin C microcapsule of the present invention, the melting temperature is 60-95°C, and after melting until completely dissolved, the microcapsule is kept warm for 10-30 minutes to make the temperature of each part consistent.

[0018] Another object of the present invention is to provide a method for preparing solid fat vitamin C microcapsules.

[0019] In order to solve the above technical problems, the present invention provides the following technical solutions: comprising:

[0020] The crushed and sieved vitamin C powder is added into the molten wall material liquid while stirring to obtain a mixed liquid;

[0021] The mixed liquid is kept warm at the melting temperature and subjected to high-speed emulsification and dispersion to obtain an emulsion;

[0022] The emulsion is granulated by spray condensation to obtain solid lipid vitamin C microcapsules.

[0023] As a preferred solution of the method for preparing the solid fat vitamin C microcapsules of the present invention, the rotation speed of the high-speed emulsification dispersion is 7000-15000 rpm, and the working time is 3-8 minutes.

[0024] As a preferred solution of the method for preparing the solid fat vitamin C microcapsules of the present invention, the spray condensation adopts a dual-fluid pressurized atomizer with a nozzle diameter of 0.7 mm and a nozzle temperature of 60-95° C., which is consistent with the melting temperature of the wall material.

[0025] As a preferred embodiment of the method for preparing solid fat vitamin C microcapsules of the present invention, the spray condensation comprises the following steps: the feed flow rate is 20-30 ml / min, the inlet and outlet temperatures in the collecting chamber are 4-6°C and 7.5-10°C respectively, and the atomizing air pressure is 0.1-0.5 MPa.

[0026] Beneficial effects of the present invention:

[0027] The solid fat vitamin C microcapsule prepared by the present invention wraps vitamin C in a hydrophobic wall material, which can effectively isolate moisture and oxygen, improve product stability, and has a controlled release effect, which can reduce the loss caused by leakage in the processing steps.

[0028] The present invention adopts the spray condensation method, which is to atomize the mixture of active substances and melted lipid materials in a cold room, avoiding a high-temperature preparation environment and having a good protective effect on heat-sensitive vitamin C.

[0029] The present invention adds liquid oil with an unsaturated structure to solid fat, and due to the difference in the size of fatty acid chains, changes the crystallization pattern, obtains soft, orderly and less β' crystals, and improves the drug-carrying capacity of the microcapsule.

[0030] The raw materials used in the invention are cheap and readily available, and the preparation method and the actual operation method are simple, and are easy to produce on a large scale. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] 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:

[0032] Figure 1 It is the chromatogram of the standard sample of vitamin C of the present invention. DETAILED DESCRIPTION

[0033] 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.

[0034] 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.

[0035] 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.

[0036] The raw materials used in the present invention are all commercially available in the art unless otherwise specified. Specifically, the solid fat used is hydrogenated palm oil, model 1801, and the specific parameters are shown in Table 1.

[0037] Table 1

[0038]

[0039]

[0040] The method for determining the encapsulation efficiency of the microcapsules prepared in the present invention is:

[0041] 1. Preparation of Vitamin C Standardized Yeast

[0042] Weigh about 0.1g (accurate to 0.01mg) of vitamin C reference substance and dilute to 100mL with 0.1% oxalic acid solution (1.4g oxalic acid dihydrate dissolved in 1000mL ultrapure water). Take 0ml, 0.05ml, 0.50ml, 1.0ml, 2.5ml, 5.0ml of the above solution and dilute to 100ml with 0.1% oxalic acid solution. The vitamin C concentrations in the standard series working solutions are 0μg / mL, 0.5μg / mL, 5.0μg / mL, 10.0μg / ml, 25.0μg / mL, 50.0μg / ml, respectively. Prepare immediately before use.

[0043] 2. Sample Solution Preparation

[0044] Vitamin C on the surface of microcapsules: Weigh 0.1g of microcapsule powder (accurate to 0.01mg), disperse it in 10mL of 0.1% oxalic acid solution with a Tween 80 content of 1g / L, vortex for 10s, and filter through a 0.45μm aqueous filter. Take 1mL of the above liquid and dilute it to 100mL with 0.1% oxalic acid solution, filter it with a 0.22μm aqueous filter, and inject it according to chromatographic conditions.

[0045] Microcapsule total vitamin C: Weigh 0.1g microcapsule powder (accurate to 0.01mg), add 10mL chloroform, shake evenly, then add 10mL 0.1% oxalic acid solution, vortex and shake for 30s to mix thoroughly, let stand to separate layers, take the supernatant, and filter through a 0.45μm aqueous filter. Take 1mL of the above liquid and dilute to 100mL with 0.1% oxalic acid solution, filter with a 0.22μm aqueous filter, and inject according to chromatographic conditions.

[0046] 3. Chromatographic conditions

[0047] a) Chromatographic column: C18 column (250mm×4.6mm×5μm)

[0048] b) Column temperature: 30℃

[0049] c) Mobile phase: 0.1% oxalic acid solution + methanol = 99 + 1

[0050] d) Flow rate: 1.0 mL / min

[0051] e) UV detection wavelength: 245nm

[0052] f) Injection volume: 20 μL

[0053] g) Injection time: 10min

[0054] 4. Analysis results and calculations

[0055] a) The content of vitamin C in the sample is calculated as follows:

[0056] X=1000C / M 样品

[0057] Where:

[0058] C——the concentration of vitamin C in the sample calculated according to the standard curve, in μg / mL;

[0059] M 样品 ——Weighing of microcapsule powder, unit: g

[0060] b) The determination of the surface vitamin C, retention rate and encapsulation rate of the obtained microcapsules is as follows:

[0061] Surface vitamin C = X 表 / X 理论 ×100%

[0062] Retention rate = X 总 / X 理论 ×100%

[0063] Encapsulation efficiency = (1-X 表 / X 总 )×100%;

[0064] Where:

[0065] X 表 ——Vitamin C content on the microcapsule surface calculated in (a)

[0066] X 总 ——The total vitamin C content of the microcapsules calculated in (a)

[0067] X 理论 ——Assuming that vitamin C does not degrade during the production process, the vitamin C content in 0.1g of microcapsule powder

[0068] Example 1

[0069] This embodiment provides a method for preparing solid fat vitamin C microcapsules, specifically:

[0070] 1) Preparation of molten wall material liquid:

[0071] 70g hydrogenated palm oil, 30g soybean oil and 1g lecithin are melted at 80°C until completely dissolved, and then kept warm for 10 minutes to make the temperatures of various parts consistent, to obtain a molten wall material liquid, wherein the mass ratio of hydrogenated palm oil to soybean oil is 7:3, and the amount of lecithin is 1% of the total mass of hydrogenated palm oil and soybean oil.

[0072] 2) Prepare the core material and wall material mixture:

[0073] Vitamin C is ground and pulverized, and passed through a 120-mesh sieve to obtain a core material, which is added to the molten wall material liquid while stirring to obtain a mixed liquid, wherein the mass ratio of the core material to the molten wall material liquid is 2:8, and the mixed liquid is always kept at the melting temperature to stabilize the temperature at 80°C, and subjected to high-speed emulsification and dispersion treatment to obtain an emulsion, wherein the high-speed emulsification disperser is set to 10000rpm, and the working time is 5min.

[0074] 3) Spray condensation:

[0075] The emulsion was spray-condensed and granulated by a dual-fluid pressurized atomizer (BUCHI, B-290). The nozzle temperature was 80°C, the feed flow rate was 25 mL / min, the inlet and outlet temperatures in the collecting chamber were 5°C and 8°C, respectively, and the atomizing air pressure was 0.3 MPa. Vitamin C microcapsules were obtained by granulation.

[0076] Example 2

[0077] This example is used to explore the effect of the ratio of solid fat to liquid oil on the encapsulation efficiency of the prepared vitamin C microcapsules. Specifically, the mass ratios of hydrogenated palm oil and soybean oil in step 1) of Example 1 were adjusted to 6:4, 7:3, 8:2, 9:1, and 10:0, respectively. The remaining steps and processes were all based on Example 1 to obtain vitamin C microcapsules with different ratios of solid fat to liquid oil in this example. The encapsulation efficiency and retention rate were tested and compared with those in Example 1. The results are shown in Table 2.

[0078] Table 2

[0079] Proportion 6:4 7:3 8:2 9:1 10:0 Surface vitamin C / % 21.71±0.28 12.59±0.7 18.57±0.89 26.53±0.88 30.1±0.85 Retention rate / % 86.91±0.28 92.88±0.70 88.83±0.91 85.80±0.90 75.19±0.86 Encapsulation rate / % 75.02±0.21 86.45±0.57 79.10±1.77 69.08±1.89 59.97±1.22

[0080] As can be seen from Table 2, as the proportion of liquid oil increases, the retention rate of vitamin C is improved to a certain extent, and the surface vitamin C content decreases, indicating that the lipids encapsulate more vitamin C. This is because the unsaturated structure in the liquid oil reduces the perfection of the lipid crystals, and the space for accommodating drug molecules becomes larger, so that more drugs can be encapsulated, which improves the retention rate and encapsulation rate of the microcapsules.

[0081] The increase in the perfection of lipid crystals makes the space for accommodating drug molecules smaller, resulting in the expulsion of encapsulated drugs, so it is necessary to form crystals with defects during production. The combination of liquid lipids and solid lipids leads to a large number of disordered crystals. The resulting lipid particle matrix exhibits large defects in the lattice and leaves enough space to accommodate drug molecules, resulting in an increase in drug loading capacity and effectively improving the encapsulation rate.

[0082] Example 3

[0083] This example is used to explore the effect of the amount of phospholipid on the encapsulation efficiency of the prepared vitamin C microcapsules. Specifically, the amount of phospholipid in step 1) of Example 1 was adjusted to 0, 0.5%, 1%, 1.5%, and 2% compared to hydrogenated palm oil and soybean oil, respectively. The remaining steps and processes were all referred to Example 1, and vitamin C microcapsules with different amounts of phospholipids in this example were obtained. The encapsulation efficiency and retention rate were tested and compared with those in Example 1. The results are shown in Table 3.

[0084] Table 3

[0085]

[0086]

[0087] It can be seen from Table 3 that as the amount of phospholipid increases, the vitamin C retention rate is improved to a certain extent, and the surface vitamin C content is reduced. The addition of phospholipid as a surfactant can promote the uniform mixing of vitamin C powder in lipids, improve the emulsification stability, and make vitamin C tend to enter the solid fat during the spray condensation process to reduce the surface tension.

[0088] Example 4

[0089] This example is used to explore the effect of the melting temperature of the molten wall material liquid on the encapsulation efficiency of the obtained vitamin C microcapsules. Specifically, the melting temperatures in step 1) of Example 1 were adjusted to 70°C, 75°C, 80°C, 85°C, and 90°C, respectively, and the remaining steps and processes were all referred to Example 1, to obtain vitamin C microcapsules with different melting temperatures in this example, and the encapsulation efficiency and retention rate were tested and compared with those in Example 1. The results are shown in Table 4.

[0090] Table 4

[0091] Melting temperature 65℃ 70℃ 75℃ 80℃ 85℃ Surface vitamin C / % 25.9±1.46 16.86±1.01 14.84±0.94 12.59±0.7 26.18±0.27 Retention rate / % 84.60±1.49 90.01±1.02 92.03±0.96 92.88±0.70 83.82±0.28 Encapsulation rate / % 69.39±2.16 81.27±0.89 83.87±1.86 86.45±0.57 68.77±2.92

[0092] As can be seen from Table 4, with the increase of lipid melting temperature, the encapsulation rate first increases and then decreases. Increasing the melting temperature can reduce the viscosity of the liquid and spray to form droplets with uniform particle size.

[0093] Example 5

[0094] This example is used to explore the effect of the core-to-wall ratio on the encapsulation efficiency of the prepared vitamin C microcapsules. Specifically, the mass ratios of the core material and the molten wall material liquid in step 2) of Example 1 were adjusted to 6:4, 5:5, 4:6, 3:7, and 2:8, respectively. The remaining steps and processes were all referred to Example 1 to obtain vitamin C microcapsules with different core-to-wall ratios of this example. The encapsulation efficiency and retention rate were tested and compared with those in Example 1. The results are shown in Table 5.

[0095] Table 5

[0096] Core-to-wall ratio 6:4 5:5 4:6 3:7 2:8 Surface vitamin C / % 17.39±0.23 12.59±0.7 20.39±1.13 22.36±1.05 25.08±0.85 Retention rate / % 90.50±0.23 92.88±0.70 90.84±1.14 87.58±1.06 85.10±0.85 Encapsulation rate / % 80.78±0.34 86.45±0.57 77.55±1.09 74.47±0.70 70.53±0.35

[0097] It can be seen from Table 5 that as the core-to-wall ratio decreases, the encapsulation first increases and then decreases. Compared with microcapsules with a small proportion of core material, microcapsules with a high core-to-wall ratio retain more vitamin C, but excessive addition of vitamin C will result in insufficient encapsulation of the microcapsules.

[0098] Example 6

[0099] This example is used to explore the effect of atomization pressure in spray condensation on the encapsulation efficiency of vitamin C microcapsules. Specifically, the atomization pressure in step 3) of Example 1 was adjusted to 0.1 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa, and 0.5 MPa, respectively. The remaining steps and processes were all referred to Example 1. Vitamin C microcapsules prepared at different feed flow rates in this example were obtained, and the encapsulation efficiency and retention rate were tested. The results were compared with those in Example 1, and the results are shown in Table 6.

[0100] Table 6

[0101] Atomization pressure / MPa 0.1 0.15 0.2 0.25 0.3 Surface vitamin C / % 18.61±1.23 14.59±0.28 8.28±0.4 11.73±0.2 12.59±0.7 Retention rate / % 89.02±1.23 91.50±0.28 93.97±0.40 92.04±0.20 92.88±0.70 Encapsulation rate / % 79.09±0.34 84.05±1.13 91.19±1.09 87.26±0.7 86.45±0.57

[0102] As can be seen from Table 6, as the atomization pressure increases, the encapsulation rate first increases and then decreases. For the same liquid, increasing the atomization pressure can reduce the liquid viscosity and form droplets with more uniform particle sizes. However, too small a particle size will lead to a large relative surface area, an increase in the surface vitamin content, and a decrease in the encapsulation rate.

[0103] In summary, the solid lipid vitamin C microcapsules prepared by the present invention encapsulate vitamin C in a hydrophobic wall material, which can effectively isolate water vapor and oxygen, improve product stability, and have a controlled release effect, which can reduce the loss caused by leakage in the processing steps.

[0104] The present invention adopts the spray condensation method, which is to atomize the mixture of active substances and melted lipid materials in a cold room, avoiding a high-temperature preparation environment and having a good protective effect on heat-sensitive vitamin C.

[0105] The present invention adds liquid oil with an unsaturated structure to solid lipids, and the combination of liquid lipids and solid lipids leads to a large number of disordered crystals. The obtained lipid particle matrix exhibits large defects on the crystal lattice, and leaves enough space to accommodate drug molecules, thereby improving the drug loading capacity and effectively improving the encapsulation rate.

[0106] The raw materials used in the invention are cheap and readily available, and the preparation method and the actual operation method are simple, and are easy to produce on a large scale.

[0107] 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 solid fat vitamin C microcapsule, characterized in that: include, Using crushed and sieved vitamin C powder as the core material; A molten wall material liquid obtained by melting solid fat, liquid oil and emulsifier is used as the wall material; The core material is wrapped by the wall material, wherein the mass ratio of the core material to the wall material is 6:4 to 2:

8.

2. The solid fat vitamin C microcapsule according to claim 1, characterized in that: The vitamin C powder is pulverized and sieved with mesh numbers ranging from 90 to 130 meshes.

3. The solid fat vitamin C microcapsule according to claim 1, characterized in that: The solid fat includes one of hydrogenated palm oil, hydrogenated rapeseed oil, stearic acid and lauric acid; The liquid oil includes one of soybean oil, peanut oil, corn oil, and oleic acid; The emulsifier includes one of phospholipids and polyglycerol ricinoleate.

4. The solid fat vitamin C microcapsule according to any one of claims 1 or 3, characterized in that: The mass ratio of the solid fat to the liquid oil is 6:4 to 10:

0.

5. The solid fat vitamin C microcapsule according to any one of claims 1 or 3, characterized in that: The amount of the emulsifier used is 0-2% of the total mass of the solid fat and the liquid oil.

6. The solid fat vitamin C microcapsule according to claim 1, characterized in that: The melting temperature is 60-95° C. After the melting is completely dissolved, the temperature is kept for 10-30 minutes to make the temperature of each part consistent.

7. The method for preparing solid fat vitamin C microcapsules according to any one of claims 1 to 6, characterized in that: include, The crushed and sieved vitamin C powder is added into the molten wall material liquid while stirring to obtain a mixed liquid; The mixed liquid is kept warm at the melting temperature and subjected to high-speed emulsification and dispersion to obtain an emulsion; The emulsion is granulated by spray condensation to obtain solid lipid vitamin C microcapsules.

8. The method for preparing solid fat vitamin C microcapsules according to claim 7, characterized in that: The rotation speed of the high-speed emulsification dispersion is 7000-15000 rpm, and the working time is 3-8 minutes.

9. The method for preparing solid fat vitamin C microcapsules according to claim 7, characterized in that: The spray condensation adopts a double-fluid pressurized atomizer, the nozzle diameter is 0.7 mm, the nozzle temperature is 60-95° C., and is consistent with the melting temperature of the wall material.

10. The method for preparing solid fat vitamin C microcapsules according to any one of claims 7 or 9, characterized in that: The spray condensation, wherein the feed flow rate is 20-30 ml / min, the inlet and outlet temperatures in the collecting chamber are 4-6° C. and 7.5-10° C. respectively, and the atomizing air pressure is 0.1-0.5 MPa.

Images