DHA algae oil oral liquid and preparation method thereof

Abstract

The invention belongs to the technical field of oral liquid, and provides DHA algae oil oral liquid and a preparation method thereof. The preparation method comprises the following steps: mixing sodium hexametaphosphate, disodium hydrogen phosphate, sodium caseinate, starch sodium octenylsuccinate and water, and refrigerating to obtain a water phase; mixing docosahexaenoic acid, caprylic capric triglyceride, essence and vitamin E oil to obtain an oil phase; adding the oil phase into the water phase, stirring at a high speed, and homogenizing the primary emulsion to obtain an embedded emulsion; and mixing the embedding emulsion, sucralose, sweet orange essence and water to obtain the DHA algae oil oral liquid. The DHA algal oil oral liquid forms a double-layer nano-emulsion structure, and the DHA algal oil nano-emulsion oral liquid with the double-layer structure has good thermal stability, freeze-thaw stability, salt, acid and alkali tolerance and long-term storage stability, and provides technical reference for development of DHA high-stability products and application of the DHA high-stability products in food processing.

Description

Technical Field

[0001] The invention relates to the technical field of oral liquids, and in particular to a DHA algae oil oral liquid and a preparation method thereof. Background Art

[0002] DHA algae oil nanoemulsion oral liquid is a nutritional supplement rich in docosahexaenoic acid (DHA). DHA is an important ω-3 long-chain polyunsaturated fatty acid that plays an important role in the intellectual and visual development of infants and young children, as well as cardiovascular and cerebrovascular health. At present, the industrialization process of DHA algae oil nanoemulsion oral liquid faces the following challenges and problems: (1) Oxidation and odor problems: The polyunsaturated fatty acid properties of DHA make it easy to oxidize and produce unpleasant flavors, which affects the sensory quality of the product and consumer acceptance. Technological innovation is needed to improve the stability of DHA algae oil and cover up unpleasant odors. (2) Stability and bioavailability: The high unsaturation of DHA leads to limitations in its transportation, storage and application. Technological innovation is needed to improve its stability and utilization rate in the human body.

[0003] At present, the industrialization technology of DHA algae oil includes microfluidization technology, which is a technology that generates high-speed fluid through tiny pores under ultra-high pressure to achieve dispersion, homogenization and emulsification. However, traditional microfluidization devices have the problems of complex operation and difficulty in continuous production.

[0004] Therefore, it is of great significance to study and obtain a DHA algae oil oral solution with improved stability and bioavailability, oxidation resistance, simple operation process and capable of continuous production. Summary of the invention

[0005] The purpose of the present invention is to provide a DHA algae oil oral liquid and a preparation method thereof in view of the deficiencies in the prior art.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The present invention provides a method for preparing a DHA algae oil oral liquid, comprising the following steps:

[0008] 1) mixing sodium hexametaphosphate, disodium hydrogen phosphate, sodium caseinate, sodium starch octenylsuccinate and water and refrigerating to obtain an aqueous phase;

[0009] 2) mixing docosahexaenoic acid, caprylic decanoic acid glyceride, essence and vitamin E oil to obtain an oil phase;

[0010] 3) adding the oil phase to the water phase and stirring at high speed to obtain colostrum; homogenizing the colostrum to obtain an embedding emulsion;

[0011] 4) Mixing the embedding emulsion, sucralose, sweet orange essence and water to obtain DHA algae oil oral solution.

[0012] Preferably, in step 1), the mass ratio of the sodium hexametaphosphate, disodium hydrogen phosphate, sodium caseinate, sodium starch octenylsuccinate and water is 0.01-0.09: 0.002-0.01: 0.1-0.9: 0.05-0.5: 20-30.

[0013] Preferably, in step 1), the mixing temperature is 45-55° C., the mixing time is 2.5-3.5 h, stirring is performed during the mixing process, and the stirring rate is 450-550 r / min; the refrigeration temperature is 4-8° C., and the refrigeration time is 10-14 h.

[0014] Preferably, in step 2), the mass ratio of docosahexaenoic acid, caprylic glyceride, essence and vitamin E oil is 0.5-5: 0.1-0.9: 0.21-1.48: 0.002-0.05; the essence comprises sweet orange oil essence, pineapple oil essence and lemon oil essence, and the mass ratio of sweet orange oil essence, pineapple oil essence and lemon oil essence is 0.1-0.5: 0.1-0.9: 0.01-0.08.

[0015] Preferably, the mixing time in step 2) is 10 to 20 minutes, and stirring is performed during the mixing process at a rate of 450 to 550 r / min.

[0016] Preferably, in the process of adding the oil phase to the water phase in step 3), the stirring rate of the water phase is 5000-8000 r / min, the high-speed stirring rate is 8000-12000 r / min, and the high-speed stirring time is 5-10 min.

[0017] Preferably, the homogenization is performed 2 to 4 times in step 3) and the homogenization pressure is 50 to 80 MPa.

[0018] Preferably, in step 3), the mass ratio of the oil phase to the water phase is 1:6-15; in step 4), the mass ratio of the embedding emulsion, sucralose, sweet orange flavor and water is 20-46: 0.006-0.02: 0.05-0.2: 53-79.

[0019] The present invention also provides a DHA algae oil oral liquid prepared by the preparation method.

[0020] The beneficial effects of the present invention include the following:

[0021] 1) The DHA algae oil oral liquid obtained by the water-in-oil method and microencapsulation technology of the present invention meets the market demand for high-quality DHA algae oil. The DHA algae oil oral liquid of the present invention forms a double-layer nanoemulsion structure, which significantly improves the stability of the emulsion; this double-layer structure can maintain the physicochemical stability of the emulsion under various environmental pressures (such as high acid and alkali, high salt, heating, freeze-thaw, etc.), thereby maintaining high stability during storage and processing (especially at high temperatures). The DHA algae oil nanoemulsion oral liquid prepared by the method of the present invention has good thermal stability, freeze-thaw stability, tolerance to salt and acid and alkali, and long-term storage stability, which provides a technical reference for the development of high-stability products of DHA and its application in food processing.

[0022] 2) Uniform particle size distribution: The preparation method of the present invention controls the content of the water phase and the oil phase and the high-pressure homogenization process, so that the obtained emulsion has a smaller particle size and a more uniform particle size distribution, which helps to improve the stability and bioavailability of the product.

[0023] 3) Oxidation protection: The structure of the nanoemulsion of the present invention provides an additional layer of protection for DHA, reducing the possibility of oxidation and extending the shelf life of the product.

[0024] 4) Masking bad flavors: DHA algae oil itself may have an unpleasant flavor. Through emulsification process and adding flavors, these bad flavors can be effectively masked and the sensory quality of the product can be improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is the particle size distribution of the DHA algae oil nanoemulsion oral solution in Example 1. DETAILED DESCRIPTION

[0026] The present invention provides a method for preparing a DHA algae oil oral liquid, comprising the following steps:

[0027] 1) mixing sodium hexametaphosphate, disodium hydrogen phosphate, sodium caseinate, sodium starch octenylsuccinate and water and refrigerating to obtain an aqueous phase;

[0028] 2) mixing docosahexaenoic acid, caprylic decanoic acid glyceride, essence and vitamin E oil to obtain an oil phase;

[0029] 3) adding the oil phase to the water phase and stirring at high speed to obtain colostrum; homogenizing the colostrum to obtain an embedding emulsion;

[0030] 4) Mixing the embedding emulsion, sucralose, sweet orange essence and water to obtain DHA algae oil oral solution.

[0031] In the present invention, the mass ratio of the sodium hexametaphosphate, disodium hydrogen phosphate, sodium caseinate, sodium starch octenylsuccinate and water in step 1) is preferably 0.01-0.09: 0.002-0.01: 0.1-0.9: 0.05-0.5: 20-30, more preferably 0.03-0.07: 0.004-0.008: 0.3-0.7: 0.1-0.4: 22-28, and more preferably 0.04-0.05: 0.005-0.006: 0.5-0.6: 0.2-0.3: 24-25.

[0032] In the present invention, the mixing temperature in step 1) is preferably 45-55°C, more preferably 47-52°C, and more preferably 50°C; the mixing time is preferably 2.5-3.5h, and more preferably 3h; stirring is preferably performed during the mixing process, and the stirring rate is preferably 450-550r / min, more preferably 480-520r / min, and more preferably 500r / min; the refrigeration temperature is preferably 4-8°C, more preferably 5-7°C, and more preferably 6°C, and the refrigeration time is preferably 10-14h, more preferably 11-13h, and more preferably 12h.

[0033] In the present invention, the mass ratio of docosahexaenoic acid, caprylic decanoic acid glyceride, essence and vitamin E oil in step 2) is preferably 0.5-5: 0.1-0.9: 0.21-1.48: 0.002-0.05, more preferably 1-4: 0.3-0.7: 0.52-1.3: 0.01-0.04, and more preferably 2-3: 0.4-0.5: 0.8-1.1: 0.0 2~0.03; the flavor preferably comprises sweet orange oil flavor, pineapple oil flavor and lemon oil flavor, and the mass ratio of sweet orange oil flavor, pineapple oil flavor and lemon oil flavor is preferably 0.1~0.5:0.1~0.9:0.01~0.08, further preferably 0.2~0.4:0.3~0.7:0.02~0.07, and more preferably 0.3:0.5~0.6:0.04~0.05.

[0034] In the present invention, the mixing time in step 2) is preferably 10 to 20 min, more preferably 12 to 18 min, and more preferably 14 to 15 min; stirring is preferably performed during the mixing process, and the stirring rate is preferably 450 to 550 r / min, more preferably 480 to 520 r / min, and more preferably 500 r / min.

[0035] In the present invention, in the process of adding the oil phase to the water phase in step 3), the stirring rate of the water phase is preferably 5000-8000 r / min, more preferably 5500-7500 r / min, more preferably 6000-7000 r / min, the high-speed stirring rate is preferably 8000-12000 r / min, more preferably 9000-11000 r / min, more preferably 10000 r / min, and the high-speed stirring time is preferably 5-10 min, more preferably 6-9 min, more preferably 7-8 min.

[0036] In the present invention, the number of homogenization in step 3) is preferably 2 to 4 times, more preferably 3 times, and the homogenization pressure is preferably 50 to 80 MPa, more preferably 55 to 75 MPa, and more preferably 60 to 70 MPa.

[0037] In the present invention, the mass ratio of the oil phase to the water phase in step 3) is preferably 1:6-15, more preferably 1:8-13, and more preferably 1:10-11; the mass ratio of the embedding emulsion, sucralose, sweet orange flavor and water in step 4) is preferably 20-46: 0.006-0.02: 0.05-0.2: 53-79, more preferably 25-40: 0.008-0.016: 0.08-0.16: 55-75, and more preferably 30-35: 0.01-0.012: 0.1-0.12: 60-70.

[0038] In the present invention, stirring, liquid medicine circulation and filtration are sequentially performed after mixing to obtain DHA algae oil oral solution; the stirring rate is preferably 40 to 60 r / min, more preferably 45 to 55 r / min, more preferably 50 r / min, the stirring time is preferably 25 to 35 min, more preferably 28 to 32 min, more preferably 30 min; the liquid medicine circulation pressure is preferably 0.1 to 0.6 MPa, more preferably 0.2 to 0.5 MPa, more preferably 0.3 to 0.4 MPa.

[0039] The present invention also provides a DHA algae oil oral liquid prepared by the preparation method.

[0040] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0041] The parts in the examples are all parts by mass.

[0042] Example 1

[0043] Add 25 parts of purified water into a shear emulsification tank, add 0.05 parts of sodium hexametaphosphate, 0.005 parts of disodium hydrogen phosphate, 0.5 parts of sodium caseinate, 0.3 parts of sodium starch octenylsuccinate, heat to 50°C, stir at 500 r / min for 3 hours, and then refrigerate at 6°C for 12 hours to obtain a uniform aqueous phase.

[0044] Place 3 parts of docosahexaenoic acid in a stainless steel barrel, add 0.5 parts of caprylic decanoic acid glyceride, 0.3 parts of sweet orange oil essence, 0.5 parts of pineapple oil essence, 0.05 parts of lemon oil essence, and 0.02 parts of vitamin E oil, and stir at a speed of 500 r / min for 15 minutes to obtain a uniform oil phase.

[0045] The oil phase was slowly added to the aqueous phase under stirring (stirring rate was 7000r / min), the mass ratio of the oil phase to the aqueous phase was 1:10, and then high-speed stirring was performed at a rate of 10000r / min for 8 minutes to obtain colostrum; the colostrum was homogenized by a high-pressure homogenizer (all the colostrum passed through the homogenization pipe once, and it was homogenized 3 times in total), the homogenization pressure was 70MPa, and an embedding emulsion was obtained.

[0046] Add the embedding emulsion, sucralose, and sweet orange essence to a 100 mL liquid preparation tank, and then add purified water (the mass ratio of embedding emulsion, sucralose, sweet orange essence, and water is 35:0.012:0.12:65) to the full volume to obtain a solution. Turn on the stirring and liquid circulation pump (stirring rate is 50r / min, stirring time is 30min, and the pressure of the liquid circulation pump is 0.3MPa), and filter the solution with a 300-mesh stainless steel filter to obtain a DHA algae oil nanoemulsion oral solution.

[0047] Example 2

[0048] Add 22 parts of purified water into a shear emulsification tank, add 0.03 parts of sodium hexametaphosphate, 0.004 parts of disodium hydrogen phosphate, 0.3 parts of sodium caseinate, and 0.1 parts of sodium starch octenylsuccinate, heat to 45°C, stir at 450 r / min for 3.5 hours, and then refrigerate at 4°C for 10 hours to obtain a uniform aqueous phase.

[0049] Place 1 part of docosahexaenoic acid in a stainless steel barrel, add 0.3 parts of caprylic decanoic acid glyceride, 0.2 parts of sweet orange oil essence, 0.3 parts of pineapple oil essence, 0.02 parts of lemon oil essence, and 0.01 parts of vitamin E oil, and stir at a speed of 450 r / min for 20 minutes to obtain a uniform oil phase.

[0050] The oil phase was slowly added to the aqueous phase under stirring (stirring rate was 6000r / min), the mass ratio of the oil phase to the aqueous phase was 1:8, and then high-speed stirring was performed at a rate of 9000r / min for 10min to obtain colostrum; the colostrum was homogenized by a high-pressure homogenizer (all the colostrum passed through the homogenization pipe once, and it was homogenized 3 times in total), the homogenization pressure was 60MPa, and an embedding emulsion was obtained.

[0051] Add the embedding emulsion, sucralose, and sweet orange essence to a 100 mL liquid preparation tank, and then add purified water (the mass ratio of the embedding emulsion, sucralose, sweet orange essence, and water is 25:0.008:0.08:55) to the full volume to obtain a solution. Turn on the stirring and liquid circulation pump (stirring rate is 45r / min, stirring time is 32min, and the pressure of the liquid circulation pump is 0.2MPa), and filter the solution with a 300-mesh stainless steel filter to obtain a DHA algae oil nanoemulsion oral solution.

[0052] Example 3

[0053] Add 28 parts of purified water into a shear emulsification tank, add 0.07 parts of sodium hexametaphosphate, 0.008 parts of disodium hydrogen phosphate, 0.7 parts of sodium caseinate, and 0.4 parts of sodium starch octenylsuccinate, heat to 55°C, stir at 550 r / min for 2.5 hours, and then refrigerate at 8°C for 14 hours to obtain a uniform aqueous phase.

[0054] Place 4 parts of docosahexaenoic acid in a stainless steel barrel, add 0.7 parts of caprylic decanoic acid glyceride, 0.4 parts of sweet orange oil essence, 0.7 parts of pineapple oil essence, 0.07 parts of lemon oil essence, and 0.04 parts of vitamin E oil, and stir at a speed of 550 r / min for 10 minutes to obtain a uniform oil phase.

[0055] The oil phase was slowly added to the aqueous phase under stirring (stirring rate was 7500r / min), the mass ratio of the oil phase to the aqueous phase was 1:13, and then high-speed stirring was performed at a rate of 11000r / min for 6 minutes to obtain colostrum; the colostrum was homogenized by a high-pressure homogenizer (all the colostrum passed through the homogenization pipe once, and it was homogenized 3 times in total), the homogenization pressure was 80MPa, and an embedding emulsion was obtained.

[0056] Add the embedding emulsion, sucralose, and sweet orange essence to a 100 mL liquid preparation tank, and then add purified water (the mass ratio of the embedding emulsion, sucralose, sweet orange essence, and water is 40:0.016:0.12:70) to the full volume to obtain a solution. Turn on the stirring and liquid circulation pump (stirring rate is 55r / min, stirring time is 28min, and the pressure of the liquid circulation pump is 0.5MPa), and filter the solution with a 300-mesh stainless steel filter to obtain a DHA algae oil nanoemulsion oral solution.

[0057] The particle size distribution of the DHA algae oil nanoemulsion oral solution of Example 1 is as follows: Figure 1 As shown, from Figure 1 It can be seen that the particle size of DHA algae oil nanoemulsion oral solution is small and the particle size distribution is narrow. The particle size distribution range is 38-59nm and the average particle size is 43nm.

[0058] The water solubility and stability of the DHA algae oil nanoemulsion oral solution prepared in Examples 1 to 3 were tested.

[0059] (1) The results of the water solubility test are as follows: the DHA algae oil nanoemulsion oral liquids of Examples 1 to 3 can be rapidly dissolved in water, and the solutions are clear, indicating that the DHA algae oil nanoemulsion oral liquids have good water solubility.

[0060] (2) Stability test:

[0061] Physical stability test:

[0062] 1) Centrifugation experiment: 30 mL of algae oil DHA nanoemulsion was placed in a centrifuge tube and centrifuged at 4000 r / min for 15 min. No stratification should be observed.

[0063] The test shows that the DHA algae oil nanoemulsion oral liquid prepared in Examples 1 to 3 has no stratification phenomenon and the stability meets the requirements.

[0064] 2) Shaking test: 30 mL of each of the DHA algae oil nanoemulsion oral liquids prepared in Examples 1 to 3 were sealed in 50 mL test tubes, placed in a 30° C. constant temperature water bath oscillator, and shaken at a rate of 100 r / min. Samples were taken at 12 h, 24 h, 48 h, and 72 h, respectively, and the centrifugal stability parameter Ke of the DHA algae oil nanoemulsion at each sampling time was determined. The results are shown in Table 1.

[0065] Table 1 Shaking test results of DHA algae oil nanoemulsion oral solution

[0066]

[0067] It can be seen from Table 1 that continuous shaking has no effect on the Ke value of DHA algae oil nanoemulsion.

[0068] 3) Temperature stability test: The DHA algae oil nanoemulsion oral liquid of Example 1 was filled in a soda-lime glass bottle and sealed, and placed at 40°C, 60°C, and 70°C for 10 days, respectively. The particle size of the DHA algae oil nanoemulsion oral liquid was tested at 0 day, 5 days, and 10 days, respectively. The results are shown in Table 2.

[0069] Table 2 Effect of different temperatures on particle size of algae oil DHA nanoemulsion

[0070]

[0071] As shown in Table 2, there is no significant change in the particle size of DHA algae oil nanoemulsion at different temperatures. Since DHA algae oil is a fat-soluble component, it should not be stored for too long at high temperature.

[0072] 4) Accelerated test: The accelerated test was carried out at 30°C. The DHA algae oil oral solution of Example 1 was placed at 30°C for 6 months. The physical properties of the DHA algae oil oral solution were examined at 0 month, 1 month, 2 months, 3 months and 6 months. The results are shown in Table 3.

[0073] Table 3 Effect of accelerated test on particle size of DHA algae oil nanoemulsion

[0074] Time / month 0 month January February March June Particle size / nm 43±10 43±10 44±10 44±10 45±10

[0075] It can be seen from Table 3 that under the accelerated test conditions, the particle size of the DHA algae oil nanoemulsion did not change significantly.

[0076] Chemical stability test:

[0077] 1) High temperature test: The DHA algae oil oral solution of Example 1 was filled in a soda-lime glass bottle and sealed, and placed at 40°C, 60°C, and 70°C for 10 days, respectively. The content changes of the components in the DHA algae oil nanoemulsion were investigated at 0 days, 5 days, and 10 days, respectively. The results are shown in Table 4.

[0078] Table 4 Component contents of DHA algae oil nanoemulsion under different temperature and time conditions

[0079]

[0080] As shown in Table 4, when the DHA algae oil nanoemulsion is placed under the above test conditions, the DHA content does not change significantly during the storage period.

[0081] 2) Accelerated test: The DHA algae oil oral solution was placed at 37°C for 6 months, and the changes in DHA content at 0, 1, 2, 3, and 6 months were examined. The results are shown in Table 5.

[0082] Table 5 Contents of components in DHA algae oil nanoemulsions after accelerated test at 37°C for 6 months

[0083]

[0084] As shown in Table 5, the content index of the components of the DHA algae oil nanoemulsion has no obvious change, and the DHA algae oil nanoemulsion has good stability.

[0085] The preparation process of the DHA algae oil nanoemulsion oral liquid of the present invention has obvious advantages in improving product stability, masking bad flavor, improving bioavailability, etc., and can effectively solve the technical problems of easy oxidation, poor stability, poor sensory quality, etc. of DHA during the application process, providing a technical basis for the wide application of DHA in the fields of food, health care products, etc.

[0086] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a DHA algae oil oral liquid, characterized in that: The steps include: 1) mixing sodium hexametaphosphate, disodium hydrogen phosphate, sodium caseinate, sodium starch octenylsuccinate and water and refrigerating to obtain an aqueous phase; 2) mixing docosahexaenoic acid, caprylic decanoic acid glyceride, essence and vitamin E oil to obtain an oil phase; 3) adding the oil phase to the water phase and stirring at high speed to obtain colostrum; homogenizing the colostrum to obtain an embedding emulsion; 4) Mixing the embedding emulsion, sucralose, sweet orange essence and water to obtain DHA algae oil oral solution.

2. The preparation method according to claim 1, characterized in that: Step 1) The mass ratio of the sodium hexametaphosphate, disodium hydrogen phosphate, sodium caseinate, sodium starch octenylsuccinate and water is 0.01-0.09: 0.002-0.01: 0.1-0.9: 0.05-0.5: 20-30.

3. The preparation method according to claim 1 or 2, characterized in that: Step 1) The mixing temperature is 45-55°C, the mixing time is 2.5-3.5 hours, stirring is performed during the mixing process, and the stirring rate is 450-550 r / min; the refrigeration temperature is 4-8°C, and the refrigeration time is 10-14 hours.

4. The preparation method according to claim 3, characterized in that: Step 2) The mass ratio of docosahexaenoic acid, caprylic glyceride, essence and vitamin E oil is 0.5-5: 0.1-0.9: 0.21-1.48: 0.002-0.05; the essence comprises sweet orange oil essence, pineapple oil essence and lemon oil essence, and the mass ratio of sweet orange oil essence, pineapple oil essence and lemon oil essence is 0.1-0.5: 0.1-0.9: 0.01-0.

08.

5. The preparation method according to claim 3, characterized in that: Step 2) The mixing time is 10 to 20 minutes, and stirring is performed during the mixing process at a rate of 450 to 550 r / min.

6. The preparation method according to claim 4 or 5, characterized in that: Step 3) During the process of adding the oil phase to the water phase, the stirring rate of the water phase is 5000-8000 r / min, the high-speed stirring rate is 8000-12000 r / min, and the high-speed stirring time is 5-10 min.

7. The preparation method according to claim 6, characterized in that: Step 3) The homogenization is performed 2 to 4 times at a pressure of 50 to 80 MPa.

8. The preparation method according to claim 7, characterized in that: In step 3), the mass ratio of the oil phase to the water phase is 1:6-15; in step 4), the mass ratio of the embedding emulsion, sucralose, sweet orange essence and water is 20-46: 0.006-0.02: 0.05-0.2: 53-79.

9. DHA algae oil oral liquid prepared by the preparation method according to any one of claims 1 to 8.

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