Lycopene micro-capsule powder and preparation method thereof
11723879 · 2023-08-15
Assignee
Inventors
- Wei Gao (Hebei, CN)
- Jianzhong Xu (Hebei, CN)
- Xiangyu Yang (Hebei, CN)
- Hong TIAN (Hebei, CN)
- Yamei Li (Hebei, CN)
- Xinchao Jia (Hebei, CN)
Cpc classification
A23L33/105
HUMAN NECESSITIES
A23P10/40
HUMAN NECESSITIES
A61K9/5161
HUMAN NECESSITIES
A61K47/22
HUMAN NECESSITIES
A61K9/1623
HUMAN NECESSITIES
A61K47/36
HUMAN NECESSITIES
International classification
A61K47/22
HUMAN NECESSITIES
A61K47/36
HUMAN NECESSITIES
Abstract
The present invention discloses a method for preparing a lycopene micro-capsule powder, wherein lycopene is fully mixed with an aqueous phase to obtain a lycopene emulsion, and the emulsion is then ground to a particle size less than 1 μm, and spray dried. The aqueous phase comprises: a gelatin enzymatic hydrolysate with a molecular weight of 5,000-10,000 Da, disaccharide, polysaccharide, and an antioxidant. The disaccharide is one or more of sucrose, maltose and lactose; and the polysaccharide is one or more of pullulan and chitosan.
Claims
1. A method for preparing lycopene micro-capsule powder, comprising: adding 1 to 2 parts of gelatin to 3 to 4 parts of water, adding protease for enzymatic hydrolysis, and boiling, and then cooling to obtain gelatin enzymatic hydrolysate with a molecular weight of 5000 to 10000 Da at a temperature of 55 to 65° C.; adding 2 to 3 parts of disaccharide, 0.3 to 0.5 parts of polysaccharide and 0.1 to 0.2 parts of antioxidant to the gelatin enzymatic hydrolysate, stirring and dissolving sufficiently at 40 to 50 r/min to obtain an aqueous phase; adding 1 part of lycopene to the aqueous phase, shearing and stirring at 7000 to 9000 r/min at 55 to 65° C. for 10 to 20 minutes to obtain a lycopene emulsion, wherein the lycopene comprises a content of 90 wt % to 92 wt %; grinding the lycopene emulsion to a particle size of less than 1 μm to obtain a lycopene microemulsion; and spray drying the lycopene microemulsion to obtain lycopene micro-capsule powder.
2. The method according to claim 1, wherein the gelatin enzymatic hydrolysate is prepared by a method comprising the following steps: adding gelatin to water, and adding protease under conditions of 55 to 65° C. and pH value of 7.5 to 8.5 for enzymatic hydrolysis, after enzymatic hydrolysis is completed, subjecting the resultant to boiling, and then cooling and keeping at the temperature of 55 to 65° C. to obtain the gelatin enzymatic hydrolysate; the protease is papain, and/or the dosage of the protease is 2.0% to 3.0% of the mass of gelatin.
3. The method according to claim 1, wherein the disaccharide is one or more selected from sucrose, maltose and lactose; and/or, the polysaccharide is one or more selected from pullulan polysaccharide and chitosan; and/or, the antioxidant is one or more selected from ascorbic acid and vitamin E.
4. The method according claim 1, wherein the mass ratio of the lycopene to gelatin contained in the aqueous phase is 1:(1-2).
5. The method according to claim 1, wherein the grinding comprises grinding to a particle size of 200 to 600 nm; the grinding is carried out by a nano-grinder at a rotation speed of 1600 to 1800 r/min for 1.0 to 2.0 h.
6. The method according to claim 1, wherein the conditions for spray drying comprises: an inlet air temperature of 165 to 180° C., an outlet air temperature of 90 to 105° C., and an air rate of 300 to 500 mL/h.
7. A lycopene micro-capsule powder prepared by the method according to claim 1.
8. The method according to claim 1, wherein the gelatin enzymatic hydrolysate is prepared by a method comprising the following steps: adding gelatin to water, and adding protease under conditions of 55 to 65° C. and pH value of 7.5 to 8.5 for enzymatic hydrolysis, after enzymatic hydrolysis is completed, subjecting the resultant to boiling, and then cooling and keeping at the temperature of 55 to 65° C. to obtain the gelatin enzymatic hydrolysate.
9. The method according to claim 1, wherein the disaccharide is one or more selected from sucrose, maltose and lactose; and/or, the polysaccharide is one or more selected from pullulan polysaccharide and chitosan; and/or, the antioxidant is one or more selected from ascorbic acid and vitamin E.
10. The method according to claim 2, wherein the disaccharide is one or more selected from sucrose, maltose and lactose; and/or, the polysaccharide is one or more selected from pullulan polysaccharide and chitosan; and/or, the antioxidant is one or more selected from ascorbic acid and vitamin E.
11. The method according claim 2, wherein the mass ratio of the lycopene to gelatin contained in the aqueous phase is 1:(1-2).
12. The method according claim 3, wherein the mass ratio of the lycopene to gelatin contained in the aqueous phase is 1:(1-2).
13. A lycopene micro-capsule powder prepared by the method according to claim 2.
14. A lycopene micro-capsule powder prepared by the method according to claim 3.
15. A lycopene micro-capsule powder prepared by the method according to claim 4.
16. A lycopene micro-capsule powder prepared by the method according to claim 5.
17. A lycopene micro-capsule powder prepared by the method according to claim 6.
Description
DETAILED DESCRIPTION OF THE INVENTION
(1) The specific embodiments of the present invention will be further described in detail in combination with Examples. The following Examples are intended to illustrate the present invention, but not intended to limit to the scope of the present invention.
Example 1
(2) The present Example provides a preparation method of lycopene micro-capsule powder, specifically comprising the following steps:
(3) (1) 150 g of gelatin was added to 225 g of purified water, and papain was added in an amount of 3.75 g. The resulting solution was adjusted to a pH of 7.5, and subjected to enzymatic hydrolysis at a temperature of 55° C. in water bath for 3 h. The resultant was boiled for 15 min, and then cooled to 55° C. to obtain a gelatin enzymatic hydrolysate. The gelatin in the gelatin enzymatic hydrolysate had a molecular weight of 7000 Da;
(4) (2) 225 g of sucrose, 22.5 g of pullulan polysaccharide, 10 g of ascorbic acid, and 5 g of vitamin E were added to the gelatin enzymatic hydrolysate, and the resultant was stirred at 65° C. at a rotation speed of 40 r/min for 45 min to obtain an aqueous phase;
(5) (3) 75 g of lycopene crystals with a content of 90 wt % was added to the aqueous phase while stirring, and the resultant was sheared at a shear speed of 9000 r/min and a temperature of 65° C. for 10 min to obtain a lycopene emulsion;
(6) (4) The lycopene emulsion was ground by a nano-grinder at a rotation speed of 1700 r/min for 1.5 h to obtain a lycopene microemulsion with a particle size of 400 nm;
(7) (5) The lycopene microemulsion was spray-dried with an inlet air temperature of 175° C., an outlet air temperature of 100° C., and a flow rate of 500 mL/h to obtain a lycopene micro-capsule powder.
Example 2
(8) The present Example provides a preparation method of lycopene micro-capsule powder, specifically comprising the following steps:
(9) (1) 200 g of gelatin was added to 437.5 g of purified water, and papain was added in an amount of 6 g. The resulting solution was adjusted to a pH of 8.0, and subjected to enzymatic hydrolysis at a temperature of 60° C. in water bath for 5 h. The resultant was boiled for 15 min, and then cooled to 60° C. to obtain a gelatin enzymatic hydrolysate. The gelatin in the gelatin enzymatic hydrolysate had a molecular weight of 8000 Da;
(10) (2) 250 g of maltose, 62.5 g of pullulan polysaccharide, 2.5 g of ascorbic acid and 10 g of vitamin E were added to the gelatin enzymatic hydrolysate, and the resultant was stirred at 60° C. at a rotation speed of 30 r/min for 50 min to obtain an aqueous phase;
(11) (3) 125 g of lycopene crystals with a content of 90 wt % was added to the aqueous phase while stirring, and the resultant was sheared at a shear speed of 8000 r/min and a temperature of 60° C. for 15 min to obtain a lycopene emulsion;
(12) (4) The lycopene emulsion was ground by a nano-grinder at a rotation speed of 1800 r/min for 1 h to obtain a lycopene microemulsion with a particle size of 500 nm;
(13) (5) The lycopene microemulsion was spray-dried with an inlet air temperature of 180° C., an outlet air temperature of 105° C., and a flow rate of 400 mL/h to obtain a lycopene micro-capsule powder.
Example 3
(14) The present Example provides a preparation method of lycopene micro-capsule powder, specifically comprising the following steps:
(15) (1) 165 g of gelatin was added to 440 g of purified water, and papain was added in an amount of 3.3 g. The resulting solution was adjusted to a pH of 8.5, and subjected to enzymatic hydrolysis at a temperature of 65° C. in water bath for 4 h. The resultant was boiled for 15 min, and then cooled to 65° C. to obtain a gelatin enzymatic hydrolysate. The gelatin in the gelatin enzymatic hydrolysate had a molecular weight of 5000 Da;
(16) (2) 275 g of lactose, 44 g of chitosan and 22 g of ascorbic acid were added to the gelatin enzymatic hydrolysate, and the resultant was stirred at 65° C. at a rotation speed of 50 r/min for 30 min to obtain an aqueous phase;
(17) (3) 110 g of lycopene crystals with a content of 90 wt % was added to the aqueous phase while stirring, and the resultant was sheared at a shear speed of 7000 r/min and a temperature of 65° C. for 20 min to obtain a lycopene emulsion;
(18) (4) The lycopene emulsion was ground by a nano-grinder at a rotation speed of 1800 r/min for 2.0 h to obtain a lycopene microemulsion with a particle size of 200 nm;
(19) (5) The lycopene microemulsion was spray-dried with an inlet air temperature of 170° C., an outlet air temperature of 95° C., and a flow rate of 300 mL/h to obtain a lycopene micro-capsule powder.
Example 4
(20) The present Example provides a preparation method of lycopene micro-capsule powder, specifically comprising the following steps:
(21) (1) 100 g of gelatin was added to 320 g of purified water, and papain was added in an amount of 2.5 g. The resulting solution was adjusted to a pH of 8.2, and subjected to enzymatic hydrolysis at a temperature of 60° C. in water bath for 3.5 h. The resultant was boiled for 15 min, and then cooled to 55° C. to obtain a gelatin enzymatic hydrolysate. The gelatin in the gelatin enzymatic hydrolysate had a molecular weight of 10000 Da;
(22) (2) 125 g of sucrose, 125 g of maltose, 20 g of pullulan polysaccharide, 15 g of chitosan, and 15 g of vitamin E were added to the gelatin enzymatic hydrolysate, and the resultant was stirred at 55° C. at a rotation speed of 45 r/min for 60 min to obtain an aqueous phase;
(23) (3) 100 g of lycopene crystals with a content of 92 wt % was added to the aqueous phase while stirring, and the resultant was sheared at a shear speed of 7500 r/min and a temperature of 55° C. for 30 min to obtain a lycopene emulsion;
(24) (4) The lycopene emulsion was ground by a nano-grinder at a rotation speed of 1600 r/min for 1.0 h to obtain a lycopene microemulsion with a particle size of 600 nm;
(25) (5) The lycopene microemulsion was spray-dried with an inlet air temperature of 165° C., an outlet air temperature of 90° C., and a flow rate of 450 mL/h to obtain a lycopene micro-capsule powder.
Comparative Example 1
(26) (1) 150 g of gelatin was added to 225 g of purified water, the resultant was boiled for 15 min, and then cooled to 55° C. to obtain a solution. The gelatin in the gelatin solution had a molecular weight of 45000 Da;
(27) (2) 225 g of sucrose, 22.5 g of pullulan polysaccharide, 10 g of ascorbic acid and 5 g of vitamin E were added to the gelatin solution, and the resultant was stirred at 65° C. at a rotation speed of 40 r/min for 45 min to obtain an aqueous phase;
(28) (3) 75 g of lycopene crystals with a content of 90 wt % was added to the aqueous phase while stirring, and the resultant was sheared at a shear speed of 9000 r/min and a temperature of 65° C. for 10 min to obtain a lycopene emulsion;
(29) (4) The lycopene emulsion was ground by a nano-grinder at a rotation speed of 1700 r/min for 1.5 h to obtain a lycopene microemulsion with a particle size of 1.2 μm;
(30) (5) The lycopene microemulsion was spray-dried with an inlet air temperature of 175° C., an outlet air temperature of 100° C., and a flow rate of 500 mL/h to obtain a lycopene micro-capsule powder.
Experimental Example 1: Chroma Comparison
(31) Three kinds of lycopene micro-capsule powder were randomly purchased from the market, and the chroma thereof was tested together with the lycopene provided in Examples 1 to 4. The test results were shown in Table 1.
(32) TABLE-US-00001 TABLE 1 Test value of chroma of lycopene micro-capsule powder L* a* b* Example 1 38.5 30.0 19.5 Example 2 40.2 29.0 20.0 Example 3 39.0 29.6 19.3 Example 4 39.4 29.3 19.7 Comparative Example 1 57.2 13.09 1.32 commercially available 23.72 8.44 4.64 product 1 commercially available 27.99 9.52 4.39 product 2 commercially available 32.13 7.89 5.07 product 3
(33) It can be seen from the results in Table 1 that, the method provided by the present invention can effectively improve the color tone of the obtained product compared with the dark red color of other products, making it brighter and more vivid.
Experimental Example 2: Stability Test
(34) The lycopene micro-capsule powders provided in Examples 1 to 4 were kept at a temperature of 25° C. and a humidity of 60% in dark for one year. The content of lycopene and chroma were tested. The test results were shown in Table 2.
(35) TABLE-US-00002 TABLE 2 Changes in content of lycopene and chroma value Direct test without storage Test after keeping for one year content of content of lycopene lycopene (wt %) L* a* b* (wt %) L* a* b* Example 1 10.94 38.5 30.0 19.5 10.75 39.6 29.4 19.9 Example 2 11.54 40.2 29.0 20.0 11.40 41.04 27.9 20.6 Example 3 11.50 39.0 29.6 19.3 11.27 40.3 28.6 19.7 Example 4 10.68 39.4 29.3 19.7 10.44 40.0 28.9 19.0 Comparative 10.90 57.2 13.09 1.32 6.65 57.9 4.8 −0.87 Example 1
(36) It can be seen from the results in Table 2 that the lycopene micro-capsule powder provided by the present invention has good stability, and there is no obvious change in the content of lycopene and chroma value after storage for one year.
(37) The above contents are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modification, equivalent replacement, improvement and the like made according to the spirit and principle of the present invention shall be regarded as within the protection scope of the invention.