Method of preparing highly stable microcapsule powders or microparticles containing fat-soluble nutrient having increased double bonds

Abstract

The present invention provides a method of preparing highly stable microcapsule powders or microparticles containing a fat-soluble nutrient having multiple double bonds. The method includes a) dissolving the fat-soluble nutrient having multiple unsaturated double bonds to prepare an oil phase; b) dissolving a part of a capsule shell material into water to prepare an aqueous phase; c) shearing the aqueous phase and the oil phase, and mixing and emulsifying the same to obtain an emulsion; d) homogenizing the emulsion by a standard high-pressure homogenizer, to make the emulsion obtain droplets in the emulsion with an average particle diameter at a nanometer level, thereby producing a nanometer scale emulsion; e) directly adding a remaining part of the capsule shell material into the homogenized nanometer scale emulsion, and shearing, mixing, and dissolving the same to obtain a twice-embedded emulsion; and f) performing spray granulation on the twice-embedded emulsion, and drying resultant granules to obtain the highly stable microcapsule powder or microparticles.

Claims

1. A method of preparing highly stable microcapsule powders or microparticles containing a fat-soluble nutrient having multiple double bonds, comprising the following steps: a) dissolving a fat-soluble nutrient having multiple unsaturated double bonds to prepare an oil phase; b) dissolving a part of a capsule shell material in water to prepare an aqueous phase; c) shearing the aqueous phase and the oil phase, and mixing and emulsifying the same to obtain an emulsion; d) homogenizing the emulsion by a standard high-pressure homogenizer to make the emulsion obtain droplets in the emulsion with an average particle diameter at a nanometer level, thereby producing a nanometer scale emulsion; e) directly adding a remaining part of the capsule shell material into the homogenized nanometer scale emulsion, and shearing, mixing and dissolving the same to obtain a twice-embedded emulsion; and f) performing spray granulation on the twice-embedded emulsion, and drying resultant granules to obtain highly stable microcapsule powders or microparticles, wherein the capsule shell material of step b) and the remaining part of the capsule shell material of step e) are the same material, and is selected from the group consisting of modified starch, gelatin, gum Arabic, and sodium caseinate.

2. The method according to claim 1, wherein the fat-soluble nutrient having multiple unsaturated double bonds is selected from the group consisting of VA, VE, natural VE, VD3, coenzymes 10, curcumin, carotenoid and polyunsaturated fatty acid.

3. The method according to claim 2, wherein the carotenoid is selected from the group consisting of beta-carotene, lutein, astaxanthin, lycopene, and zeaxanthin; the polyunsaturated fatty acid is derived from a source selected from the group consisting of animal extract oil, fermented source and a synthetic source; the polyunsaturated fatty acid is selected from the group consisting of conjugated linoleic acid, arachidonic acid, linoleic acid, linolenic acid, eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and a mixture thereof.

4. The method according to claim 1, wherein the aqueous phase or the oil phase further comprises an antioxidant.

5. The method according to claim 4, wherein the antioxidant is selected from the group consisting of vitamin C, ascorbyl palmitate, mixed tocopherols, synthetic tocopherols, sodium ascorbate, and rosemary.

6. The method according to claim 1, wherein in step b) an amount of the capsule shell material in the aqueous phase is in a range of 15-85 wt. % of the total amount of the capsule shell material, when preparing the aqueous phase.

7. The method according to claim 1, wherein, in the process of high pressure homogenization of step d), a temperature of the emulsion after homogenizing is increased no more than 10 C. relative to a temperature of pre-homogenizing.

8. The method according to claim 1, wherein in the process of high pressure homogenization of step d) a homogenization pressure is in a range of 10 MPa to 40 MPa.

Description

DETAILED DESCRIPTION AND PREFERRED EMBODIMENTS THEREOF

(1) Hereafter, the present invention will be described specifically with reference to the examples. The examples are given only for illustration of the technical solution of the present invention and should not be construed to limit the present invention.

Example 1

(2) Mix 48 g of fish oil -3 fatty acid ethyl ester (EPA 33.5%, DHA 23.1%, total content of -3 PUFA is 59.8%) with 2 g of mixed tocopherols to form a solution, and stir the solution at 30 C. until homogeneous to obtain an oil phase.

(3) Add 10 g of modified starch to 80 ml water, and raise the temperature to 40 C., and fully stir and dissolve to obtain an aqueous phase.

(4) Add the aqueous phase to a shear tank, and shear and stir, at the same time slowly add the oil phase to the aqueous phase, to make the oil phase and the aqueous phase fully shear, mix and emulsify, to obtain an emulsion. The emulsion temperature should be 52 C. and the viscosity of the emulsion should be 8.5 cPa after completion of the emulsification. The emulsion is then homogenized by a high Pressure Homogenizer (made by Changzhou homogeneous Machinery Co., Ltd. Type: GJB1000-80, homogenization pressure: 30 MPa). After homogenization, the temperature of the emulsion is up to 59 C. (the increased temperature is 7 C., the average particle diameter of the emulsion droplet measured by a laser particle size distribution instrument is 580 nm.

(5) Add 20 g modified starch to the homogenized emulsion under shearing and stirring for 10 min, to form a twice-embedded emulsion outside the emulsion droplets after the modified starch is completely dissolved, to finally obtain 160 g of the emulsion and the solid content is 50 wt %; and then obtain fish oil -3 fatty acid ethyl ester microcapsule microparticles by a common technique of spray starch bed fluidized drying (20 g modified starch is absorbed), wherein the polyunsaturated fatty acids content is 26.5%.

(6) The fish oil -3 fatty acid ethyl ester microcapsule microparticles have good dispersibility in water, with the average particle diameter being 633 nm of the emulsion droplet. The microparticles after tabletting the microparticles under a pressure 250 MPa still have good stability. The microcapsule microparticles are sealed in an aluminum foil bag. The stability data of the sealed microcapsule microparticles at 40 C. is provided in Table 1.

(7) The obtained microcapsule microparticles are placed in a jar, and then odors are measured by using an electronic nose, a quantitative value of the electronic nose is 23.5. Afterwards the jar is kept in a water bath at 60 C. for 10 min, and then odors are measured by using an electronic nose again, and a quantitative value of the electronic nose is 27.6. The odor change of the microcapsule microparticles is found to be less.

Comparative Example 2

(8) Mix 48 g fish oil -3 fatty acid ethyl ester (EPA 33.5%, DHA 23.1%, total content of -3 PUFA is 59.8%) with 2 g mixed tocopherols to form a solution, and stir the solution at 30 C. until homogeneous to obtain an oil phase.

(9) Add 30 g modified starch to 100 ml water, raise the temperature to 40 C., and stir and dissolve to obtain an aqueous phase.

(10) Add the aqueous phase to a shear tank, and shear and stir, at the same time slowly add the oil phase to the aqueous phase, to make the oil phase and the aqueous phase fully shear, mix and emulsify, to obtain an emulsion. The emulsion temperature was at 45 C. and the viscosity of the emulsion was 90 cPa after completion of the emulsification. The emulsion is then homogenized by a high Pressure Homogenizer with a homogenization pressure of 50 MPa. After homogenization, the temperature of the emulsion was 72 C. (the increase in temperature was 27 C.) the average particle diameter of the emulsion droplet measured by a laser particle size distribution instrument was 1380 nm.

(11) Finally, obtain 180 g of the emulsion and the solid content is 44.5 wt %; and then obtain fish oil -3 fatty acid ethyl ester microcapsule microparticles by a common technique of spray starch bed fluidized drying (25 g modified starch is absorbed), wherein the polyunsaturated fatty acids content is 24.7%.

(12) The fish oil -3 fatty acid ethyl ester microcapsule microparticles have good dispersibility in water, with an average particle diameter of 1420 nm of the emulsion droplet. The microparticles after tableting the microparticles under a pressure 250 MPa have poor stability. The microcapsule microparticles are sealed in an aluminum foil bag. The stability data of the sealed microcapsule microparticles at 40 C. is listed in Table 1.

(13) The obtained microcapsule microparticles are placed in a jar, and then the odor level is measured by using an electronic nose, with a quantitative value of the electronic nose being 89.3. Afterwards the jar is kept in a water bath at 60 C. for 10 minutes, and then odors were again measured by using the electronic nose, and a quantitative value of the electronic nose was 223.8. The odors of the microcapsule microparticles were found to be very strong and were especially so after heating.

(14) It may be seen by comparison that the viscosity of the emulsion of Example 1 is still lower in the case of adding less water due to add a small amount of capsule shell materials before homogenization. After the emulsion is homogenized at a relatively low pressure, the average particle diameter of the emulsion droplet is only 500 nm. Moreover, the emulsion temperature is increased less (only increased by 7 C.). Therefore it would have less damage to the stablity of the fish oil -3 PUFA, no new low molecular material is produced. Therefore the final products are kept without fishy odors being produced during storage. The average particle diameter of the emulsion droplet in the final microcapsule microparticles is 630 nm. The smaller particle diameter emulsion droplet are beneficial to the stability of the final products. Further, subsequently adding the capsule shell materials can form a twice-embedded emulsion, so as to further be beneficial to the stablity of the microcapsule microparticles. After high pressure tableting, the microcapsule microparticles were stored for 3 months and the retention rate was still found to be more than 87%.

(15) On the contrary, in Comparative Example 2, adding at once the capsule shell materials before high pressure homogenization makes the viscosity of the emulsion higher and increases the homogenization pressure. However, the average particle diameter of the emulsion droplet is whereas micron-scale. And the homogenization time is extended and the homogenization temperature is obviously increased during homogenization up to 27 C. It makes parts of the polyunsaturated fatty acids degrade and produce strong fishy odors. Moreover, the stability of the final product and tabletted product are obviously less than that of Example 1.

(16) TABLE-US-00001 TABLE 1 Stability Comparison of fish oil -3 fatty acid ethyl ester microcapsule microparticies and tabletted product obtained by different processes (sealed in aluminium foil bag at 40 C.) Example 1 Example 2 microparticles tabletted microparticles tabletted Time Retention Retention Retention Retention (month) content rate content rate content rate content rate 0 26.5% 100% 26.5% 100% 24.7% 100% 24.7% 100% 1 25.8% 97.4% 24.4% 92.1% 22.4% 90.5% 21.0% 85.0% 2 25.2% 95.2% 23.4% 88.4% 21.7% 87.8% 19.6% 79.8% 3 24.9% 94.0% 23.2% 87.7% 21.1% 85.6% 18.7% 75.9%

Example 3

(17) Mix 20 g lutein crystals (total content of carotenoids is 87.5%, wherein the ratio of zeaxanthin is 13.2%) with 4.5 g synthetic tocopherols, and heat to 180 C. until melting to form an oil phase.

(18) Add 35 g gelatin to 210 ml water, and fully dissolve at a temperature to 40 C. to obtain an aqueous phase, and add ascorbic acid sodium to the aqueous phase to obtain an aqueous phase.

(19) Slowly add the oil phase to the aqueous phase under shearing, and fully shear, mix and emulsify the oil phase and the aqueous phase for 10 minutes to obtain an emulsion. The viscosity of the emulsion is 120 cPa. The emulsion is then homogenized by a Homogenizer, the homogenization pressure is 25 MPa. After homogenization, the temperature of the emulsion is 72 C. (the increased temperature is 5 C.) the average particle diameter of the emulsion droplet measured by a laser particle size distribution instrument is 158 nm.

(20) 35 g gelatin and 64 g sucrose are added to the homogenized emulsion in the case of shearing, and continue to shear and mix for 10 minutes to obtain lutein microcapsule dry powders containing zeaxanthin by spray drying.

(21) Dissolve the lutein microcapsule powders in water to obtain the emulsion with 164 nm particle diameter. The lutein microcapsule powders have good stability. The retention rate of the tabletted lutein microcapsule powders after tabletting is still more than 85% in the case of open storage at 40 C. for 3 months.

Examples 4-9

(22) TABLE-US-00002 TABLE 2 The implement objects and related parameters of Examples 4-9 Example 3 Example 4 Example 5 Example6 Example 7 Example 8 Example 9 Type and Quantity 12 g 45 g 10 g 15 g 15 g 21 g algae 15 g vitamin of active ingredients conjugated curcumin astaxanthin, coenzymes arachidonic DHA A, 30 g linoleic 10 g Q10, 25 g acid (AA), vitamin E, acid, lycopene, reduced 5 g linolenic 2 g vitamin 3 g linoleic 5 g beta- Coenzyme D3, 30 g acid carotenes Q10 natural vitamin E pre-addition amount 15 g 85 g 9.0 g 30 g 10 g 50 g 10 g of capsule shell gum Arabic gelatin modified sodium modified modified gelatin material starch caseinate starch starch Quantity of water 50 ml 150 ml 150 ml 90 ml 60 ml 180 ml 70 ml added in aqueous phase Antioxidant 4.0 g 6.0 g 3.0 g 4.0 g 2.0 g 9.0 g 3.5 g lecithin vitamin C ascorbyl sodium rosemary ascorbyl mixed palmitat ascorbate palmitat tocopherols Viscosity of emulsion 4.5 7.9 5.4 9.4 2.1 3.2 5.6 before homogenization (cPa) Homogenization 20 MPa 30 MPa 25 MPa 25 MPa 10 MPa 20 MPa 40 MPa pressure Increased temperature 6 C. 10 C. 6 C. 9 C. 4 C. 5 C. 7 C. during the homogeni- zation additional amount 26 g 15 g 51.0 g 30.0 g 35 g 150 g 10 g of capsule shell material average particle 345 nm 790 nm 370 nm 685 nm 420 nm 520 nm 730 nm diameter of emulsion droplet Drying mode Fluid bed Fluid bed Fluid bed Spray drying Freeze Spray drying Fluid bed spray spray spray drying drying spray drying drying drying retention rate of 91.2% 94.6% 96.2% 93.2% 93.7% 92.6% 90.0% microcapsule product after storing for 3 month retention rate of 85.0% 92.5% 93.5% 87.9% 84.9% 89.2% 88.5% tabletted microcapsule product after storing for 3 month

(23) The experiment of the present invention shows that the microcapsule powders or microparticles prepared by the method of the present invention have good stability.

(24) The present invention as illustrated by the above examples, however, should understand that the present invention is not limited to the special instance and implementation scheme described herein. These special examples and implementation plans are aimed at helping the person skilled in the art to practice the present invention. The person skilled in the art is easily able from the spirit and scope of the present invention to further improve and perfect, so the present invention only is restricted by the content and scope of the claims of the present invention, and its intention to cover all in the alternative solutions and equivalent solutions which are included in the appended claims without limiting the scope of the invention.