FAT-SOLUBLE NUTRIENT MICROCAPSULE AND PREPARATION METHOD THEREOF

Abstract

The present invention discloses a fat-soluble nutrient microcapsule and a preparation method thereof. The fat-soluble nutrient microcapsule comprises the following components in percentage by weight: a fat-soluble nutrient (0.2-51.6%), an antioxidant (0.2-5.0%), a wall material (41.4-97.6%) and a moisture (2.0-5.0%) and the ratio of the fat-soluble nutrient that keeps active in the fat-soluble nutrient microcapsule to the fat-soluble nutrient that is initially added is 0.990-0.997:1. The preparation method of the fat-soluble nutrient microcapsule comprises an emulsification process and a granulation process, wherein the emulsification is performed in a cavitation emulsifier. By the preparation method, the nutrient active substance of the fat-soluble nutrient microcapsule has less lost and high stability.

Claims

1. A fat-soluble nutrient microcapsule, comprising the following components in percentage by weight: TABLE-US-00009 a fat-soluble nutrient 0.2-51.6%; an antioxidant 0.2-5.0%; a wall material 41.4-97.6%; and water 2.0-5.0%; wherein the ratio of the fat-soluble nutrient that keeps active in the fat-soluble nutrient microcapsule to the fat-soluble nutrient that is initially added is 0.990-0.997:1.

2. The fat-soluble nutrient microcapsule according to claim 1, characterised in that the fat-soluble nutrient is selected one or more from vitamin A derivatives, vitamin E derivatives, vitamin D, carotenoid, and coenzyme Q.sub.10.

3. The fat-soluble nutrient microcapsule according to claim 2, characterised in that the fat-soluble nutrient is selected one or more from vitamin A acetate, vitamin A palmitate, vitamin E acetate, vitamin E palmitate, vitamin D2, vitamin D3, -carotenoid, astaxanthin, lycopene, canthaxanthus, lutein and coenzyme Q10.

4. The fat-soluble nutrient microcapsule according to claim 1, characterised in that the antioxidant is selected one or more from propyl gallate, BHT, tea polyphenol, -tocopherol, L-ascorbic acid-6-palmitate, tea polyphenol palmitate, sodium ascorbate, ascorbic acid, dilauryl thiodipropionate and lipoic acid; and preferably, the antioxidant is a water-soluble antioxidant comprising one or more of ascorbic acid, sodium ascorbate, erythorbic acid, and sodium erythorbate.

5. The fat-soluble nutrient microcapsule according to claim 1, characterised in that the wall material consists of a water-soluble colloid and a carbohydrate.

6. The fat-soluble nutrient microcapsule according to claim 5, characterised in that the water-soluble colloid is selected one or more from gelatin, gum arabic, gelatinizable modified starch, and starch octenyl succinate; and the carbohydrate is selected one or more from dextrin, glucose, white granulated sugar, fructose, maltose, inositol, and corn starch.

7. A preparation method of the fat-soluble nutrient microcapsule according to claim 1, comprising: emulsifying or dispersing a molten fat-soluble nutrient oil phase or pre-dispersion containing a fat-soluble core material and an aqueous phase containing a water-soluble wall material by mixing or passing respectively into a multistage series cavitation emulsifier under a high pressure to obtain an emulsion solution or a dispersion solution, and getting a fat-soluble nutrient microcapsule by spray granulation and drying of the obtained emulsion solution or dispersion solution.

8. The preparation method of the fat-soluble nutrient microcapsule according to claim 7, characterised in that the multistage series cavitation emulsifier is a series cavitation emulsifier with more than three stages; and preferably the multistage series cavitation emulsifier is a 5 to 10-stage series cavitation emulsifier.

9. The preparation method of the fat-soluble nutrient microcapsule according to claim 7, characterised in that, each stage of the cavitation emulsifier consists of a contraction section and an expansion section which are in communication, and an outlet of the constriction section and an outlet of the expansion section do not overlap entirely or partially in an outlet direction of the constriction section.

10. The preparation method of the fat-soluble nutrient microcapsule according to claim 7, characterised in that the high pressure is 100-500 MPa.

Description

DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS

[0016] The fat-soluble nutrient of the present invention is vitamin A derivatives, vitamin E derivatives, vitamin D, carotenoid, or coenzyme Q. Preferably, the fat-soluble nutrient is an unstable nutrient, and specifically may be one of vitamin A acetate, vitamin A palmitate, vitamin E acetate, vitamin E palmitate, vitamin D2, vitamin D3, and beta-carotene, astaxanthin, lycopene, canthaxanthin, lutein, and coenzyme Q10.

[0017] The antioxidant of the present invention is selected one or more from propyl gallate, BHT, tea polyphenol, -tocopherol, L-ascorbic acid-6-palmitate, tea polyphenol palmitate, sodium ascorbate, ascorbic acid, dilauryl thiodipropionate and lipoic acid. Preferably, the antioxidant is a water-soluble antioxidant, and may be selected one or more from ascorbic acid, sodium ascorbate, erythorbic acid, and sodium erythorbate. A choice of the water-soluble antioxidant is beneficial to reduce the amount of oil phase in the process of emulsification or dispersion, increase the embedding rate of the microcapsule, reduce the amount of the oil phase exposed on the surface of the microcapsule, and improve the stability of the fat-soluble nutrient in spray granulation and drying stages.

[0018] The wall material of the present invention consists of water-soluble colloid and a carbohydrate. The water-soluble colloid is selected one or more from gelatin, gum arabic, gelatinizable modified starch, and starch octenyl succinate. The carbohydrate is selected one or more from dextrin, glucose, white granulated sugar, fructose, maltose, inositol, and corn starch.

[0019] The present invention further provides a preparation method of the above-mentioned fat-soluble nutrient microcapsule, comprising emulsifying or dispersing a molten fat-soluble nutrient oil phase or pre-dispersion containing a fat-soluble core material and an aqueous phase containing a water-soluble wall material by mixing or passing respectively into a multistage series cavitation emulsifier under a high pressure, to obtain an emulsion solution or a dispersion solution, and getting a fat-soluble nutrient microcapsule by spray granulation and drying of the obtained emulsion solution or dispersion solution. The molten fat-soluble nutrient oil phase refers to a liquid oil phase of the fat-soluble nutrient obtained at a temperature higher than a melting point of the fat-soluble nutrient. The pre-dispersion of the fat-soluble nutrient refers to a nutrient solid suspension obtained by putting the fat-soluble nutrient into water and dispersing them uniformly by grinding or similar methods.

[0020] The multistage series cavitation emulsifier described above refers to an emulsifier in which a plurality of cavitation emulsifiers having abrupt contraction-expansion cross sections are used in series. The cavitation emulsifier is composed of a contraction section and an expansion section which are in communication with each other. In each stage of the emulsifier, the fluid first passes through the contraction section and then enters the expansion section. In the cavitation emulsifier, an outlet of the constriction section and an outlet of the expansion section do not overlap entirely or partially in an outlet direction of the constriction section. The inner diameter of the constriction section is reduced abruptly (and not closed), and the fluid performs a high velocity in the constriction section that is significantly higher than that of an inlet of the constriction section and reaches a maximum at the junction of the constriction section and the expansion section. The fluid collides with a wall of the expansion section at a high speed, causing cavitation, thereby achieving an emulsification or dispersion effect. The multistage series cavitation emulsifier is a series cavitation emulsifier with more than three stages. In the present invention, the multistage series cavitation emulsifier is selected according to the physical properties of the fat-soluble nutrient, particularly the viscosity of the melting oil or the pre-dispersion of the fat-soluble nutrient and the water-soluble wall material solution. Preferably, the multistage series cavitation emulsifier is a 5 to 10-stage series cavitation emulsifier.

[0021] In the present invention, homogeneous emulsification or dispersion can be completed in a very short time by allowing a liquid to pass through a multistage series cavitation emulsifier at a high velocity under a high pressure. The high pressure is 100-500 MPa. Under the high pressure, an outlet velocity of the fluid in the contraction section of the cavitation emulsifier reaches a maximum value and hits against on a wall surface of the expansion section, thereby forming a plurality of cavitation emulsification or dispersion, which can be emulsified or dispersed in one time in a short time.

[0022] The above oil phase is a molten fat-soluble nutrient or pre-dispersion without adding additional fat or organic solvent. In the preparation process of the microcapsule, there is a small contact surface of the fat-soluble nutrient which is in contact with the external environment, and combining with the above-mentioned emulsification or dispersion method, the prepared microcapsule has high active ingredients, and the active ingredients are almost lost nothing during the preparation process.

[0023] The above preparation method can be carried out under the protection of nitrogen. The use of nitrogen protection can eliminate the effects of oxygen in the environment on the nutrients and ensure the stability of the fat-soluble nutrient during the preparation of the microcapsule.

[0024] The moisture used in the above aqueous phase can be deoxidized in advance to further eliminate the influence of oxygen in the environment and to improve the stability of the fat-soluble nutrient during the preparation of the microcapsule. In the aqueous phase, the mass ratio of the hydrophilic wall material to the moisture is from 0.5-1:1.

[0025] The above drying process may be spray drying, spray granulation-fluidization drying or the like.

[0026] The present invention will be described in further detail by the way of specific embodiments. However, the invention is not limited to the embodiments described below.

A First Embodiment

A Vitamin A Microcapsule and Preparation Thereof

[0027] The vitamin A microcapsule comprises the following components:

TABLE-US-00002 a vitamin A acetate 360 Kg; a vitamin C 20 Kg; a gelatin 300 Kg; a glucose 100 Kg; and a dextrin 110 Kg.

[0028] 360 Kg of the vitamin A acetate crystal was weighed accurately, put into a melt kettle, and heated up to melt all the materials to get the melting oil. 1000 L of drinking water was put into a batching kettle, and then 300 Kg of gelatin, 100 Kg of glucose, 20 Kg of vitamin C, and 110 Kg of dextrin were added into the batching kettle to get a mixture. The mixture was heated and stirred to obtain a hydrosol solution. A pump was used to pump the melting oil in the melt kettle and the hydrosol solution in the batching kettle into a 5-stage series cavitation emulsifier with adjusting the pressure of the cavitation emulsifier to 400 Mpa, to perform a continuous emulsification, such that the vitamin A acetate emulsion at the outlet was obtained. The emulsion was continuously passed into a spray granulation tower sprayed with corn starch to granulate, and then fluidized and dried to obtain a vitamin A acetate microparticle. The content of each component was determined as shown in the Table 1, and a retention rate of the vitamin A acetate during the production process was calculated to be 99.7%. The vitamin A acetate microparticle was placed at 25 C. to carry out a stability test. After 6 months, the vitamin A acetate content in the microparticle was measured, and the retention rate of vitamin A acetate was calculated to be 98.2% after 6 months.

A Second Embodiment: A Vitamin D3 Microcapsule and Preparation Thereof

[0029] The vitamin D3 microcapsule comprises the following components:

TABLE-US-00003 a vitamin D3 55 Kg; a BHT 5 Kg; a gelatin 150 Kg; a glucose 200 Kg; and a dextrin 630 Kg.

[0030] 55 Kg of vitamin D3 oil was put into a melt kettle, 5 Kg of BHT was then added into the melt kettle and heated up to melt all the materials to get the melting oil. 980 L of drinking water was put into a batching kettle, and then 200 Kg of glucose, 150 Kg of gelatin, and 630 Kg of dextrin were added into the batching kettle to get a mixture. The mixture was heated and stirred to obtain a hydrosol solution. A pump was used to pump the melting oil in the melt tank and the hydrosol solution in the batching kettle into a 4-stage series cavitation emulsifier with adjusting the pressure of the cavitation emulsifier to 200 Mpa, to perform a continuous emulsification, such that the vitamin D3 emulsion at the outlet was obtained. The emulsion was continuously passed into a spray drying tower for spray drying to obtain a dry powder of vitamin D3. The content of each component of the dry powder of vitamin D3 was determined as shown in the Table 1, and a retention rate of the vitamin D3 during the production process was calculated to be 99.2%. The dry powder of vitamin D3 was placed at 25 C. to carry out a stability test. After 6 months, the content of the vitamin D3 in the dry powder of vitamin D3 was measured, and the retention rate of vitamin D3 was calculated to be 98.5% after 6 months.

A Third Embodiment A Lutein Microcapsule and Preparation Thereof

[0031] The lutein microcapsule comprises the following components:

TABLE-US-00004 a lutein 5.3 Kg; a VC sodium 5 Kg a sodium octenyl succinate 190 Kg a fructose 60 Kg; and a dextrin 250 kg.

[0032] 5.3 Kg of lutein crystal and 30 Kg of moisture (water) were put into a ball mill and ground to 5 m or less to obtain a pre-dispersion. 1050 L of drinking water was put into a batching kettle and 190 Kg of sodium octenyl succinate, 60 Kg of glucose, 250 Kg of dextrin, and 5 Kg of

[0033] VC sodium were added into the batching kettle to get a mixture. The mixture was heated and stirred to obtain a hydrosol solution. The above pre-dispersion was mixed with the hydrosol solution under stirring to obtain a dispersion. A pump was used to pump the dispersion into a 6-stage series cavitation emulsifier with adjusting the pressure of the cavitation emulsifier to 500 Mpa, to perform a continuous dispersion, such that the lutein dispersion at the outlet was obtained. The lutein dispersion was continuously passed into a spray drying tower for spray drying to obtain a dry powder of lutein. The content of each component of the dry powder of lutein was determined as shown in the Table 1, and a retention rate of the lutein during the production process was calculated to be 99.6%. The dry powder of the lutein was placed at 25 C. to carry out a stability test. After 6 months, the content of the lutein in the dry powder of lutein was measured, and the retention rate of lutein was calculated to be 99.2% after 6 months.

A First Comparative Embodiment: A Vitamin A Microcapsule and Preparation Thereof

[0034] The vitamin A microcapsule comprises the following components:

TABLE-US-00005 a vitamin A acetate 360 Kg; a tocopherol 20 Kg; a gelatin 300 Kg; a glucose 100 Kg; and a dextrin 110 Kg.

[0035] 20 Kg of the tocopherol was weighed accurately, put into a melt kettle, 360 Kg of the vitamin A acetate crystal was added into the melt kettle and heated up to melt all the materials to get the melting oil. 1000 L of drinking water was put into a batching kettle, and then 300 Kg of gelatin, 100 Kg of glucose, and 110 Kg of dextrin were added into the batching kettle to get a mixture. The mixture was heated and stirred to obtain a hydrosol solution. The vitamin A acetate melting oil in the melt kettle was added dropwise to the batching kettle, and sheared at a high speed for 20 minutes to obtain an emulsion. The emulsion was passed through a spray granulation tower to granulate, and then fluidized and dried to obtain the vitamin A acetate particles. The content of each component of the vitamin A acetate particles was determined as shown in the Table 1, and a retention rate of the vitamin A acetate during the production process was calculated to be 94.2%. The vitamin A was placed at 25 C. to carry out a stability test. After 6 months, the vitamin A acetate content in the vitamin A acetate particles was measured, and the retention rate of vitamin A acetate was calculated to be 88.1% after 6 months.

A Second Comparative Embodiment: A Vitamin D3 Microcapsule and Preparation Thereof

[0036] The vitamin D3 microcapsule comprises the following components:

TABLE-US-00006 a vitamin D3 55 Kg; a BHT 5 Kg; a gelatin 150 Kg; a glucose 200 Kg; and a dextrin 630 Kg.

[0037] 55 Kg of vitamin D3 oil was put into a melt kettle, 5 Kg of BHT was then added into the melt kettle and heated up to melt all the materials to get the melting oil. 980 L of drinking water was put into a batching kettle, and then 200 Kg of glucose, 150 Kg of gelatin, and 630 Kg of dextrin were added into the batching kettle to get a mixture. The mixture was heated and stirred to obtain a hydrosol solution. The vitamin D3 oil was added dropwise to the batching kettle, and sheared at a high speed for 20 minutes to obtain an emulsion. The emulsion was continuously passed into a spray drying tower for spray drying to obtain a dry powder of vitamin D3. The content of each component of the dry powder of vitamin D3 was determined as shown in the Table 1, and a retention rate of the vitamin D3 during the production process was calculated to be 96.5%. The dry powder of vitamin D3 was placed at 25 C. to carry out a stability test. After 6 months, the content of the vitamin D3 in the dry powder of vitamin D3 was measured, and the retention rate of vitamin D3 was calculated to be 93.5% after 6 months.

A Third Comparative Embodiment: A Lutein Microcapsule and Preparation Thereof

[0038] The lutein microcapsule comprises the following components:

TABLE-US-00007 a lutein 5.3 Kg; a tocopherol 5 Kg a gelatinizable modified starch 190 Kg a fructose 60 Kg; and a dextrin 250 kg.

[0039] 5.3 Kg of tocopherol was put into a melt kettle, 5.3 Kg of lutein crystal was then added into the melt kettle and heated to 180 C. to melt all the materials and then cooled down to 90 C. to get the melting oil. 1050 L of drinking water was put into a batching kettle and 190 Kg of the gelatinizable modified starch, 60 Kg of the glucose, and 250 Kg of dextrin were added into the batching kettle to get a mixture. The mixture was heated and stirred to obtain a hydrosol solution. The above lutein melting oil was added dropwise to the batching kettle, and sheared at a high speed for 20 minutes to obtain an emulsion. The lutein emulsion was sprayed into a spray drying tower to obtain a dry powder of lutein. The content of each component of the dry powder of lutein was determined as shown in the Table 1, and a retention rate of the lutein during the production process was calculated to be 75.6%. The dry powder of lutein was placed at 25 C. to carry out a stability test. After 6 months, the content of the lutein in the dry powder of lutein was measured, and the retention rate of lutein was calculated to be 72.2% after 6 months.

Forth-Tenth Embodiments

[0040] The group distribution ratio, the series of the cavitation emulsifier and pressure were according to Table 1, and the preparation process was according to the second embodiment (fourth, fifth and tenth embodiments) or the third embodiment (sixth, seventh, eighth and ninth embodiments) to obtain different nutrient microcapsules. The content of each component of the nutrient microcapsule was determined as shown in the Table 1, and the retention and stability of the nutrients thereof were calculated. The results were shown in Table 1.

TABLE-US-00008 TABLE 1 Retention rate of different formula nutrient microcapsules in the production process and storage at 25 C. for 6 months Retention Series of rate after Fat- Cavitation Retention storage at soluble Anti- emulsifier rate during 25 C. for nutrient/ oxidant/ Wall moisture/ (pressure/ production/ 6 months/ Items % % material/% % Mpa) % % The first vitamin vitamin gelatin 2.01 5 99.7 98.2 embodi- A C 29.4 (400) ment acetate 1.96 glucose 35.27 9.8 dextrin 10.77 corn starch 10.78 The vitamin BHT gelatin 2.88 4 99.2 98.5 second D3 0.47 14.01 (200) embodi- 5.08 glucose ment 18.68 dextrin 58.82 The lutein VC sodium 3.19 6 99.6 99.2 third 1.01 sodium octenyl (500) embodi- 0.95 succinate ment 37.01 fructose 11.38 dextrin 47.43 The vitamin L- gum arabic 3.51 6 99.0 98.3 fourth A ascorbic 26.08 (350) embodi- palmitate acid-6- sucrose ment 21.03 palmitate 24.23 5.05 dextrin 21.00 The vitamin Lipoic octenyl 2.09 3 99.7 99.5 fifth E acid succinate (100) embodi- acetate 0.21 starch ment 51.63 46.07 the sixth lycopene dilauroyl gelatinizable 2.77 4 99.3 98.6 embodi- 0.20 thiodipro- modified (180) ment pionate starch 0.31 40.67 ascorbic maltodextrin acid 25.58 0.94 sucrose 29.53 the - propionate gum arabic 2.53 10 99.7 98.8 seventh carotene gallate 46.22 (500) embodi- 10.33 1.02 white sugar ment sodium 18.04 ascorbate dextrin 1.10 20.76 the canthax sodium gelatin 4.98 6 99.2 98.3 eighth anthin erythorbate 42.23 (450) embodi- 11.32 3.26 dextrin ment 18.57 inositol 19.64 the astaxanthin erythorbic gelatin 2.28 7 99.5 99.2 ninth 11.27 acid 55.06 (480) embodi- 2.35 maltose ment 15.08 dextrin 13.96 the tenth coenzyme - octenyl 3.98 9 99.2 98.9 embodi- Q10 tocopherol succinate (380) ment 2.32 1.23 starch vitamin 63.5.7 E maltodextnn acetate 23.89 5.01 The first vitamin - gelatin 2.19 none 94.2 88.1 compar- A tocopherol 29.34 ative acetate 1.96 glucose embodi- 35.21 9.78 ment dextrin 10.75 cornstarch 10.77 The vitamin BHT gelatin 2.85 none 96.5 93.5 second D3 0.47 14.01 compar- 5.08 white sugar ative 18.68 embod- dextrin iment 58.85 The lutein tocopherol gelatinizable 3.32 none 75.6 72.2 third 1.01 0.95 modified compar- starch ative 35.99 embod- fructose iment 11.37 dextrin 47.36