CN112471512A - High-stability beta-carotene microcapsule and preparation method thereof - Google Patents
High-stability beta-carotene microcapsule and preparation method thereof Download PDFInfo
- Publication number
- CN112471512A CN112471512A CN202011459525.3A CN202011459525A CN112471512A CN 112471512 A CN112471512 A CN 112471512A CN 202011459525 A CN202011459525 A CN 202011459525A CN 112471512 A CN112471512 A CN 112471512A
- Authority
- CN
- China
- Prior art keywords
- carotene
- beta
- container
- pectin
- mixing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OENHQHLEOONYIE-UKMVMLAPSA-N all-trans beta-carotene Natural products CC=1CCCC(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C OENHQHLEOONYIE-UKMVMLAPSA-N 0.000 title claims abstract description 61
- 235000013734 beta-carotene Nutrition 0.000 title claims abstract description 61
- TUPZEYHYWIEDIH-WAIFQNFQSA-N beta-carotene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C)C=CC=C(/C)C=CC2=CCCCC2(C)C TUPZEYHYWIEDIH-WAIFQNFQSA-N 0.000 title claims abstract description 61
- 239000011648 beta-carotene Substances 0.000 title claims abstract description 61
- 229960002747 betacarotene Drugs 0.000 title claims abstract description 61
- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 title claims abstract description 61
- 239000003094 microcapsule Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000002156 mixing Methods 0.000 claims abstract description 53
- 235000010987 pectin Nutrition 0.000 claims abstract description 51
- 229920001277 pectin Polymers 0.000 claims abstract description 51
- 239000001814 pectin Substances 0.000 claims abstract description 51
- 239000003921 oil Substances 0.000 claims abstract description 41
- 235000019198 oils Nutrition 0.000 claims abstract description 41
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 37
- 238000001816 cooling Methods 0.000 claims abstract description 25
- 108010046377 Whey Proteins Proteins 0.000 claims abstract description 23
- 102000007544 Whey Proteins Human genes 0.000 claims abstract description 23
- 239000008055 phosphate buffer solution Substances 0.000 claims abstract description 23
- 235000021119 whey protein Nutrition 0.000 claims abstract description 23
- 239000004471 Glycine Substances 0.000 claims abstract description 19
- 238000001694 spray drying Methods 0.000 claims abstract description 18
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 11
- 239000003549 soybean oil Substances 0.000 claims abstract description 11
- 238000004108 freeze drying Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 238000007711 solidification Methods 0.000 claims abstract description 9
- 230000008023 solidification Effects 0.000 claims abstract description 9
- 239000012071 phase Substances 0.000 claims description 81
- 239000000203 mixture Substances 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 235000005979 Citrus limon Nutrition 0.000 claims description 21
- 244000131522 Citrus pyriformis Species 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 claims description 10
- 150000001746 carotenes Chemical class 0.000 claims description 10
- 235000005473 carotenes Nutrition 0.000 claims description 10
- 238000004945 emulsification Methods 0.000 claims description 10
- 239000000839 emulsion Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- NCYCYZXNIZJOKI-UHFFFAOYSA-N vitamin A aldehyde Natural products O=CC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C NCYCYZXNIZJOKI-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 abstract description 6
- 235000015097 nutrients Nutrition 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 229940045997 vitamin a Drugs 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/045—Organic compounds containing nitrogen as heteroatom
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/231—Pectin; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Nutrition Science (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Botany (AREA)
- Mycology (AREA)
- General Preparation And Processing Of Foods (AREA)
- Jellies, Jams, And Syrups (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a preparation method of a high-stability beta-carotene microcapsule, which comprises the following steps: (1) mixing pectin, glycine, pericarpium Citri Junoris-fructus Citri Limoniae extract and water in a container, sealing the container, heating to 55 + -5 deg.C, pressurizing, and keeping the temperature; reducing pressure, and rapidly cooling to below-30 deg.C for solidification; balancing the air pressure inside and outside the container, taking out the coagulum, freeze-drying to constant weight, and standing to normal temperature to obtain the processed pectin; (2) uniformly mixing the treated pectin and the whey protein, and preserving heat at the temperature of 40-70 ℃ to obtain a wall material A; (3) dissolving a wall material A in a PBS (phosphate buffer solution) with the pH = 4.5-5.5 to obtain a water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; (4) dispersing; (5) homogenizing; (6) spray drying to obtain the beta-carotene microcapsule. The beta-carotene microcapsule prepared by the processing technology of the invention greatly reserves the nutrient components and effectively improves the stability.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a high-stability beta-carotene microcapsule and a preparation method thereof.
Background
Beta-carotene is a natural pigment, antioxidant and precursor of high-effective vitamin A, and is a safe and harmless food additive. However, β -carotene in its natural state has a very low solubility in water due to the presence of its conjugated unsaturated double bonds, is very unstable in structure, and is susceptible to degradation and isomerization at mild, aerobic and high temperatures (> 50 ℃), which greatly limits its application in the food and medical fields.
The microcapsule technology is a technology for embedding solid small particles, liquid small droplets or gas by using a continuous film formed by a material wall material compounded by one or more substances by a physical, chemical or physicochemical method. The microcapsule has functional characteristics mainly depending on wall material, so as to improve the characteristics of the core material, and the microcapsule technology is proved to be an effective method for protecting sensitive substances to light, temperature, oxygen and humidity, realizing the stability and the storage resistance of active compounds and overcoming the transportation property. The stability and the biological accessibility of the beta-carotene are improved, and the beta-carotene is hopeful to be realized by a microcapsule technology.
Disclosure of Invention
The invention provides a preparation method of a high-stability beta-carotene microcapsule, which comprises the following steps:
(1) mixing pectin, glycine, orange peel-lemon extract and water in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is heated to the temperature to ensure that the internal pressure of the container is more than or equal to 3 standard atmospheric pressures, and then preserving heat for 3-6 hours; after the heat preservation is finished, pumping the air pressure in the container to be less than or equal to 0.3 standard atmospheric pressure, and then rapidly cooling to below-30 ℃ for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ or below to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein, and preserving the heat of the mixture for 10-15 h at the relative humidity of 60-80% and the temperature of 40-70 ℃ to obtain a wall material A;
(3) dissolving the wall material A in a PBS (phosphate buffer solution, solute solubility of 0.01 mol/L, and adjusting to a required pH value by using 10wt% of sodium hydroxide aqueous solution or 10wt% of dilute hydrochloric acid, wherein the PBS adopted in the invention has the concentration) with the pH = 4.5-5.5 to obtain a water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C;
(4) dispersing: uniformly mixing the oil phase and the water phase, and stirring for 1-4 min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: and (3) carrying out spray drying on the homogenized solution to obtain the beta-carotene microcapsule.
Further, the preparation method of the orange peel-lemon extract comprises the following steps: mixing dry orange peels and fresh lemon pulps, chopping, putting the mixture into ethanol, carrying out water bath at constant temperature of 60 +/-5 ℃, carrying out constant-temperature extraction for 2-4 h, carrying out air cooling to normal temperature after extraction, filtering, and carrying out liquid phase concentration under reduced pressure until no alcohol smell exists, thus obtaining the orange peel-lemon extract.
Further, the mixing mass ratio of the dry orange peels to the fresh lemon pulps is =1: 0.2-0.8; the solid-liquid mass ratio of the mixture of the dried orange peels and the lemon pulps in the ethanol solution is 1: 5-6.
Further, in the step (1), the mixing mass ratio of pectin, glycine, orange peel-lemon extract and water is pectin: glycine: orange peel-lemon extract: water =10: 0.08-0.14: 1-3: 80-100; the cooling speed is 8-10 ℃/5 min.
Further, the mixing mass ratio of the pectin to the whey protein after treatment is pectin/whey protein =1: 3.5-4.5.
Further, the mass volume fraction of the wall material A in the water phase B is 1-2%, and the mass volume fraction of the wall material A in the oil phase C is 1-2%β-the mass fraction of carotene is 0.05% -0.15%.
Further, the mixing mass ratio of the oil phase to the water phase is =1: 8.5-9.5.
Therefore, the beneficial effects of the invention are as follows: the beta-carotene microcapsule prepared by the processing technology of the invention greatly reserves the nutrient components and effectively improves the stability.
Drawings
FIG. 1 is a graph comparing the stability of the prepared beta-carotene microcapsules with untreated beta-carotene for each experimental group.
Detailed Description
The following is a detailed description with reference to examples:
example 1
A preparation method of high-stability beta-carotene microcapsules comprises the following steps:
(1) mixing pectin, glycine, orange peel-lemon extract and water according to the mass ratio of pectin: glycine: orange peel-lemon extract: mixing water =10:0.08:1:80 in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is heated to the temperature to enable the internal pressure of the container to be 3 standard atmospheric pressures, and then preserving the heat for 3 hours; after the heat preservation is finished, pumping the air pressure in the container to 0.3 standard atmospheric pressure, and then rapidly cooling to-30 ℃ at a cooling speed of 10 ℃/5min for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein according to the mass ratio of pectin/whey protein =1:3.5, and preserving the temperature of the mixture for 10 hours at 70% of humidity and 60 ℃ to obtain a wall material A;
(3) dissolving wall material A in PBS (phosphate buffer solution) with pH =5 to obtain water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of the wall material A in the water phase B is 1 percent, and the oil phase C isβ-the mass fraction of carotene is 0.05%;
(4) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:8.5, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: and (3) carrying out spray drying on the homogenized solution to obtain the beta-carotene microcapsule.
The preparation method of the orange peel-lemon extract comprises the following steps: mixing dry orange peel and fresh lemon pulp according to the mass ratio of dry orange peel/fresh lemon pulp =1:0.2, chopping, putting the mixture into ethanol, and mixing the solid-liquid mass ratio of the mixture/ethanol =1: 5; keeping the temperature of the water bath constant to 60 +/-5 ℃, extracting at the constant temperature for 2 hours, cooling the mixture to the normal temperature in air after the extraction is finished, filtering, and concentrating the liquid phase under reduced pressure until no alcohol smell exists to obtain the orange peel-lemon extract.
Example 2
A preparation method of high-stability beta-carotene microcapsules comprises the following steps:
(1) mixing pectin, glycine, orange peel-lemon extract and water according to the mass ratio of pectin: glycine: orange peel-lemon extract: mixing water =10:0.1:2:90 in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is warmed to make the internal pressure of the container reach 3 standard atmospheric pressures, and then preserving the heat for 5 hours; after the heat preservation is finished, pumping the air pressure in the container to 0.3 standard atmospheric pressure, and then rapidly cooling to-30 ℃ at a cooling speed of 10 ℃/5min for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein according to the mass ratio of pectin/whey protein =1:4, and preserving the temperature of the mixture for 10 hours at 70% of humidity and 60 ℃ to obtain a wall material A;
(3) dissolving wall material A in PBS (phosphate buffer solution) with pH =5 to obtain water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of the wall material A in the water phase B is 1 percent, and the oil phase C isβ-the mass fraction of carotene is 0.1%;
(4) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:9, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: and (3) carrying out spray drying on the homogenized solution to obtain the beta-carotene microcapsule.
The preparation method of the orange peel-lemon extract comprises the following steps: mixing dry orange peel and fresh lemon pulp according to the mass ratio of dry orange peel/fresh lemon pulp =1:0.4, chopping, putting the mixture into ethanol, and mixing the solid-liquid mass ratio of the mixture/ethanol =1: 5; keeping the temperature of the water bath constant to 60 +/-5 ℃, extracting at the constant temperature for 3h, cooling the mixture to the normal temperature after the extraction is finished, filtering, and concentrating the liquid phase under reduced pressure until no alcohol smell exists to obtain the orange peel-lemon extract.
Example 3
A preparation method of high-stability beta-carotene microcapsules comprises the following steps:
(1) mixing pectin, glycine, orange peel-lemon extract and water according to the mass ratio of pectin: glycine: orange peel-lemon extract: mixing water =10:0.12:2:90 in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is warmed to make the internal pressure of the container reach 3 standard atmospheric pressures, and then preserving the heat for 5 hours; after the heat preservation is finished, pumping the air pressure in the container to 0.3 standard atmospheric pressure, and then rapidly cooling to-30 ℃ at a cooling speed of 10 ℃/5min for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein according to the mass ratio of pectin/whey protein =1:4, and preserving the temperature of the mixture for 10 hours at 70% of humidity and 60 ℃ to obtain a wall material A;
(3) dissolving wall material A in PBS (phosphate buffer solution) with pH =5 to obtain water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of the wall material A in the water phase B is 2 percent, and the oil phase C isβ-the mass fraction of carotene is 0.1%;
(4) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:9, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: and (3) carrying out spray drying on the homogenized solution to obtain the beta-carotene microcapsule.
The preparation method of the orange peel-lemon extract comprises the following steps: mixing dry orange peel and fresh lemon pulp according to the mass ratio of dry orange peel/fresh lemon pulp =1:0.6, chopping, putting the mixture into ethanol, and mixing the solid-liquid mass ratio of the mixture/ethanol =1: 6; keeping the temperature of the water bath constant to 60 +/-5 ℃, extracting at the constant temperature for 3h, cooling the mixture to the normal temperature after the extraction is finished, filtering, and concentrating the liquid phase under reduced pressure until no alcohol smell exists to obtain the orange peel-lemon extract.
Example 4
A preparation method of high-stability beta-carotene microcapsules comprises the following steps:
(1) mixing pectin, glycine, orange peel-lemon extract and water according to the mass ratio of pectin: glycine: orange peel-lemon extract: mixing water =10:0.14:3:100 in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is warmed to make the internal pressure of the container reach 3 standard atmospheric pressures, and then preserving heat for 6 hours; after the heat preservation is finished, pumping the air pressure in the container to 0.3 standard atmospheric pressure, and then rapidly cooling to-30 ℃ at a cooling speed of 10 ℃/5min for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein according to the mass ratio of pectin/whey protein =1:4.5, and preserving the temperature of the mixture for 10 hours at 70% of humidity and 60 ℃ to obtain a wall material A;
(3) dissolving wall material A in PBS (phosphate buffer solution) with pH =5 to obtain water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of the wall material A in the water phase B is 2 percent, and the oil phase C isβ-the mass fraction of carotene is 0.15%;
(4) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:9.5, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: and (3) carrying out spray drying on the homogenized solution to obtain the beta-carotene microcapsule.
The preparation method of the orange peel-lemon extract comprises the following steps: mixing dry orange peel and fresh lemon pulp according to the mass ratio of dry orange peel/fresh lemon pulp =1:0.8, chopping, putting the mixture into ethanol, and mixing the solid-liquid mass ratio of the mixture/ethanol =1: 6; keeping the temperature of the water bath constant to 60 +/-5 ℃, extracting at the constant temperature for 4 hours, cooling the mixture to the normal temperature in air after the extraction is finished, filtering, and concentrating the liquid phase under reduced pressure until no alcohol smell exists to obtain the orange peel-lemon extract.
Comparative example 1
A preparation method of a beta-carotene microcapsule comprises the following steps:
(1) mixing pectin, glycine, orange peel extract and water according to the mass ratio of pectin: glycine: orange peel extract: mixing water =10:0.1:2:90 in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is warmed to make the internal pressure of the container reach 3 standard atmospheric pressures, and then preserving the heat for 5 hours; after the heat preservation is finished, pumping the air pressure in the container to 0.3 standard atmospheric pressure, and then rapidly cooling to-30 ℃ at a cooling speed of 10 ℃/5min for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein according to the mass ratio of pectin/whey protein =1:4, and preserving the temperature of the mixture for 10 hours at 70% of humidity and 60 ℃ to obtain a wall material A;
(3) dissolving wall material A in PBS (phosphate buffer solution) with pH =5 to obtain water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of the wall material A in the water phase B is 1 percent, and the oil phase C isβ-the mass fraction of carotene is 0.1%;
(4) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:9, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: the homogenized solution was spray dried to obtain the beta-carotene microcapsules of this comparative example.
The preparation method of the orange peel extract comprises the following steps: cutting dried orange peels, placing the cut dried orange peels into ethanol, wherein the solid-liquid mass ratio of the orange peels to the ethanol is =1: 5; keeping the temperature of the water bath constant to 60 +/-5 ℃, extracting at the constant temperature for 3h, cooling the mixture to the normal temperature in air after the extraction is finished, filtering, and concentrating the liquid phase under reduced pressure until no alcohol smell exists to obtain the orange peel extract.
Comparative example 2
A preparation method of a beta-carotene microcapsule comprises the following steps:
(1) uniformly mixing pectin and whey protein according to the mass ratio of pectin/whey protein =1:4, and preserving the temperature of the mixture for 10 hours at 70% of humidity and 60 ℃ to obtain a wall material A;
(2) dissolving wall material A in PBS (phosphate buffer solution) with pH =5 to obtain water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of the wall material A in the water phase B is 1 percent, and the oil phase C isβ-the mass fraction of carotene is 0.1%;
(3) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:9, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(4) homogenizing: homogenizing the dispersed emulsion;
(5) spray drying: the homogenized solution was spray dried to obtain the beta-carotene microcapsules of this comparative example.
Comparative example 3
A preparation method of a beta-carotene microcapsule comprises the following steps:
(1) dissolving pectin in PBS solution with pH =5 to obtain aqueous phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of pectin in the water phase B is 1%, and the mass volume fraction of pectin in the oil phase C isβ-the mass fraction of carotene is 0.1%;
(2) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:9, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(3) homogenizing: homogenizing the dispersed emulsion;
(4) spray drying: the homogenized solution was spray dried to obtain the beta-carotene microcapsules of this comparative example.
Comparative example 4
A preparation method of a beta-carotene microcapsule comprises the following steps:
(1) mixing pectin, glycine, lemon extract and water according to the mass ratio of pectin: glycine: lemon extract: mixing water =10:0.1:2:90 in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is warmed to make the internal pressure of the container reach 3 standard atmospheric pressures, and then preserving the heat for 5 hours; after the heat preservation is finished, pumping the air pressure in the container to 0.3 standard atmospheric pressure, and then rapidly cooling to-30 ℃ at a cooling speed of 10 ℃/5min for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein according to the mass ratio of pectin/whey protein =1:4, and preserving the temperature of the mixture for 10 hours at 70% of humidity and 60 ℃ to obtain a wall material A;
(3) dissolving wall material A in PBS (phosphate buffer solution) with pH =5 to obtain water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C; wherein the mass volume fraction of the wall material A in the water phase B is 1 percent, and the oil phase C isβ-the mass fraction of carotene is 0.1%;
(4) dispersing: uniformly mixing the oil phase and the water phase according to the mass ratio of the oil phase to the water phase =1:9, and stirring for 3min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: and (3) carrying out spray drying on the homogenized solution to obtain the beta-carotene microcapsule.
The preparation method of the lemon extract in the comparative example comprises the following steps: cutting fresh lemon pulp, placing in ethanol after cutting, wherein the solid-liquid mass ratio of the broken lemon blocks to the ethanol is =1: 5; and (3) carrying out constant temperature extraction in a water bath to 60 +/-5 ℃ for 3h, cooling to normal temperature after extraction is finished, filtering, and concentrating the liquid phase under reduced pressure until no alcohol smell exists to obtain the lemon extract of the comparative example.
Example 5
Beta-carotene stability evaluations were performed on the beta-carotene microcapsules prepared in examples 1 to 4 and comparative examples 1 to 4 using an ultraviolet spectrophotometer. The evaluation method comprises the following steps: after leaving the β -carotene microcapsules for 7 days, they were dissolved in a 0.01 mol/L PBS solution (pH 5) together with an untreated sample (freshly prepared β -carotene), and the sample (1 mL) was extracted with a mixture of 2 mL of ethanol and 3 mL of n-hexane. After shaking the mixture thoroughly, the hexane phase was removed. The extraction was repeated twice and the hexane phases were combined. After appropriate dilution with n-hexane, the absorbance was measured at 450 nm with an ultraviolet-visible spectrophotometer. The concentration of beta-carotene was obtained by referring to a standard curve of beta-carotene prepared under the same conditions. The stability of the β -carotene microcapsules was expressed as: c (t)/C0, wherein C (t) and C0 indicate the beta-carotene content after 7 days and of the freshly prepared microcapsules, respectively. The results are shown in FIG. 1, using β -carotene that was not microencapsulated as a control.
As can be seen from fig. 1, the wall material obtained by the method of the present invention has higher stability after subsequent dispersion, homogenization and spraying. Comparing comparative example 2 and comparative example 3, it can be seen that the whey protein treatment of the wall material has a synergistic effect, so that the embedding effect of the wall material subjected to whey protein treatment on beta-carotene is better and the prepared beta-carotene has higher stability compared with the untreated wall material.
The technical solutions provided by the present invention are described in detail above, and for those skilled in the art, the ideas according to the embodiments of the present invention may be changed in the specific implementation manners and the application ranges, and in summary, the content of the present description should not be construed as limiting the present invention.
Claims (7)
1. A preparation method of high-stability beta-carotene microcapsules is characterized by comprising the following steps:
(1) mixing pectin, glycine, orange peel-lemon extract and water in a container, sealing the container, heating the mixture to 55 +/-5 ℃, introducing nitrogen into the container after the mixture is heated to the temperature to ensure that the internal pressure of the container is more than or equal to 3 standard atmospheric pressures, and then preserving heat for 3-6 hours; after the heat preservation is finished, pumping the air pressure in the container to be less than or equal to 0.3 standard atmospheric pressure, and then rapidly cooling to below-30 ℃ for solidification; balancing the air pressure inside and outside the container, taking out the solidified substance, freeze-drying at-30 ℃ or below to constant weight, and standing in the air to normal temperature to obtain the processed pectin;
(2) uniformly mixing the treated pectin and the whey protein, and preserving the heat of the mixture for 10-15 h at the relative humidity of 60-80% and the temperature of 40-70 ℃ to obtain a wall material A;
(3) dissolving a wall material A in a PBS (phosphate buffer solution) with the pH = 4.5-5.5 to obtain a water phase B; dissolving beta-carotene in soybean oil to obtain an oil phase C;
(4) dispersing: uniformly mixing the oil phase and the water phase, and stirring for 1-4 min at a high speed by using a high-speed emulsification dispersion machine;
(5) homogenizing: homogenizing the dispersed emulsion;
(6) spray drying: and (3) carrying out spray drying on the homogenized solution to obtain the beta-carotene microcapsule.
2. The preparation method of the high-stability beta-carotene microcapsule according to claim 1, characterized in that the preparation method of the orange peel-lemon extract comprises the following steps: mixing dry orange peels and fresh lemon pulps, chopping, putting the mixture into ethanol, carrying out water bath at constant temperature of 60 +/-5 ℃, carrying out constant-temperature extraction for 2-4 h, carrying out air cooling to normal temperature after extraction, filtering, and carrying out liquid phase concentration under reduced pressure until no alcohol smell exists, thus obtaining the orange peel-lemon extract.
3. The preparation method of the high-stability beta-carotene microcapsule according to claim 2, characterized in that the mixing mass ratio of the dry orange peel to the fresh lemon pulp is dry orange peel/fresh lemon pulp =1: 0.2-0.8; the solid-liquid mass ratio of the mixture of the dried orange peels and the lemon pulps in the ethanol solution is 1: 5-6.
4. The method for preparing the high-stability beta-carotene microcapsule according to claim 3, wherein in the step (1), the mixing mass ratio of pectin, glycine, orange peel-lemon extract and water is as follows: glycine: orange peel-lemon extract: water =10: 0.08-0.14: 1-3: 80-100; the cooling speed is 8-10 ℃/5 min.
5. The method for preparing the high-stability beta-carotene microcapsule according to claim 3, wherein the mixing mass ratio of the processed pectin to the whey protein is pectin/whey protein =1: 3.5-4.5.
6. The method for preparing beta-carotene microcapsule with high stability according to claim 3, wherein the mass volume fraction of the wall material A in the water phase B is 1-2%, and the oil phase C isβ-the mass fraction of carotene is 0.05% -0.15%.
7. The preparation method of the high-stability beta-carotene microcapsule according to claim 3, wherein the mixing mass ratio of the oil phase to the water phase is =1: 8.5-9.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011459525.3A CN112471512B (en) | 2020-12-13 | 2020-12-13 | High-stability beta-carotene microcapsule and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011459525.3A CN112471512B (en) | 2020-12-13 | 2020-12-13 | High-stability beta-carotene microcapsule and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112471512A true CN112471512A (en) | 2021-03-12 |
| CN112471512B CN112471512B (en) | 2022-11-08 |
Family
ID=74917449
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011459525.3A Active CN112471512B (en) | 2020-12-13 | 2020-12-13 | High-stability beta-carotene microcapsule and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112471512B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114259954A (en) * | 2021-12-31 | 2022-04-01 | 厦门大学 | Preparation method of chitosan-whey protein isolate gel for encapsulating beta-carotene |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008063158A2 (en) * | 2006-10-31 | 2008-05-29 | William Marsh Rice University | Method for nanoencapsulation |
| WO2009039472A1 (en) * | 2007-09-20 | 2009-03-26 | Kellogg Company | Crisp, filled foods and methods related thereto |
| CN103976371A (en) * | 2014-06-03 | 2014-08-13 | 中国农业大学 | Method for extracting ponkan dietary fibers through extrusion modification and enzymolysis coupling |
| CN103976353A (en) * | 2014-04-24 | 2014-08-13 | 武汉星辰现代生物工程有限公司 | Beta-carotene microcapsule production method |
| CN105747216A (en) * | 2016-03-03 | 2016-07-13 | 广州市食品工业研究所有限公司 | Microcapsules-beta and carotene powder and preparation method thereof |
| CN105876792A (en) * | 2016-04-19 | 2016-08-24 | 东北农业大学 | Preparation method of novel beta-carotene microcapsules |
| US20170087199A1 (en) * | 2016-02-10 | 2017-03-30 | Senomyx, Inc. | Compositions for delivering a cooling sensation |
| US20170143022A1 (en) * | 2015-11-20 | 2017-05-25 | Senomyx, Inc. | Compositions Incorporating an Umami Flavor Agent |
| US20190282516A1 (en) * | 2019-04-01 | 2019-09-19 | Jxtg Nippon Oil & Energy Corporation | Carotenoid-containing composition |
| WO2019243869A1 (en) * | 2018-06-19 | 2019-12-26 | Perprin S.R.L. | Protective agent for food products and the like and for curing and/or storage rooms of the same |
| WO2020230090A1 (en) * | 2019-05-14 | 2020-11-19 | Nokha Trading Llp | Ferrous sulphate oral compositions |
-
2020
- 2020-12-13 CN CN202011459525.3A patent/CN112471512B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008063158A2 (en) * | 2006-10-31 | 2008-05-29 | William Marsh Rice University | Method for nanoencapsulation |
| WO2009039472A1 (en) * | 2007-09-20 | 2009-03-26 | Kellogg Company | Crisp, filled foods and methods related thereto |
| CN103976353A (en) * | 2014-04-24 | 2014-08-13 | 武汉星辰现代生物工程有限公司 | Beta-carotene microcapsule production method |
| CN103976371A (en) * | 2014-06-03 | 2014-08-13 | 中国农业大学 | Method for extracting ponkan dietary fibers through extrusion modification and enzymolysis coupling |
| US20170143022A1 (en) * | 2015-11-20 | 2017-05-25 | Senomyx, Inc. | Compositions Incorporating an Umami Flavor Agent |
| US20170087199A1 (en) * | 2016-02-10 | 2017-03-30 | Senomyx, Inc. | Compositions for delivering a cooling sensation |
| CN105747216A (en) * | 2016-03-03 | 2016-07-13 | 广州市食品工业研究所有限公司 | Microcapsules-beta and carotene powder and preparation method thereof |
| CN105876792A (en) * | 2016-04-19 | 2016-08-24 | 东北农业大学 | Preparation method of novel beta-carotene microcapsules |
| WO2019243869A1 (en) * | 2018-06-19 | 2019-12-26 | Perprin S.R.L. | Protective agent for food products and the like and for curing and/or storage rooms of the same |
| US20190282516A1 (en) * | 2019-04-01 | 2019-09-19 | Jxtg Nippon Oil & Energy Corporation | Carotenoid-containing composition |
| WO2020230090A1 (en) * | 2019-05-14 | 2020-11-19 | Nokha Trading Llp | Ferrous sulphate oral compositions |
Non-Patent Citations (4)
| Title |
|---|
| 杨小兰，等: "纳米微胶囊技术在功能食品中的应用研究进展", 《食品科学》 * |
| 王迪，等: "β-胡萝卜素乳状液研究进展", 《中国食品添加剂》 * |
| 许朵霞，等: "蛋白质-多糖复合物对β-胡萝卜素乳液的影响", 《食品研究与开发》 * |
| 郭维图，等: "陈皮苷微波连续提取产业化试验", 《机电信息》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114259954A (en) * | 2021-12-31 | 2022-04-01 | 厦门大学 | Preparation method of chitosan-whey protein isolate gel for encapsulating beta-carotene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112471512B (en) | 2022-11-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101519624B (en) | Cinnamon essential oil microcapsule and preparation method thereof | |
| CN104887583B (en) | A kind of preparation method of cellulose base Polyphenols natural anti-oxidation compound | |
| CN101057636A (en) | Production method for water tolerance food micro capsule | |
| CN109589883A (en) | A kind of preparation method of plants essential oil powder microcapsules | |
| EP0982038B1 (en) | Stable powdery vitamin and carotenoide containing compositions and process to prepare them | |
| CN105942525A (en) | Olive oil microcapsule powder and preparation method thereof | |
| CN106072623A (en) | A kind of preparation method of composite Nano emulsion | |
| CN104824651A (en) | High-content krill oil microcapsules and preparation technology thereof | |
| CN105495272B (en) | A kind of preparation method of the molten type rosemary antioxidant of grease two | |
| CN107897915A (en) | A kind of lotus seed protein pectin complex emulsions for loading curcumin and its preparation method and application | |
| CN112471512B (en) | High-stability beta-carotene microcapsule and preparation method thereof | |
| CN114271499B (en) | Microcapsule powder with high embedding rate and preparation method thereof | |
| CN110999988A (en) | Preparation method of white tea and tea seed oil microcapsules | |
| CN111686093A (en) | Curcumin microcapsule and preparation method and application thereof | |
| CN108030063A (en) | A kind of preparation method of the beta carotene microcapsules of high carrying capacity high bioavilability | |
| CN114190507A (en) | Method for preparing essential oil microcapsules by taking cassava starch alcohol-free esterification mixture as wall material | |
| CN114431467A (en) | Food-grade carotenoid nano capsule product and preparation method thereof | |
| Tarigan et al. | Microencapsulation of Vitamin E from palm fatty acid distillate with galactomannan and gum acacia using spray drying method | |
| CN107674451A (en) | A kind of Blueberry pigment microcapsules and preparation method thereof | |
| CN104194936A (en) | Fennel essential oil microcapsule and preparation method thereof | |
| CN107468669B (en) | Preparation method of gastrodin micro-capsule granules | |
| CN113045785A (en) | Preparation method of antibacterial preservative film loaded with nanoscale essential oil | |
| CN112998273A (en) | Microemulsion and microcapsule for embedding vitamin E and algae oil and preparation method thereof | |
| CN103013796B (en) | Easily carried powder white wine and preparation method thereof | |
| CN111296729A (en) | Water-soluble astaxanthin product and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |