CN114682180A - Natural astaxanthin water-soluble microcapsule and preparation method thereof - Google Patents
Natural astaxanthin water-soluble microcapsule and preparation method thereof Download PDFInfo
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- CN114682180A CN114682180A CN202210228055.2A CN202210228055A CN114682180A CN 114682180 A CN114682180 A CN 114682180A CN 202210228055 A CN202210228055 A CN 202210228055A CN 114682180 A CN114682180 A CN 114682180A
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- water
- natural astaxanthin
- astaxanthin
- oil phase
- capsule wall
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- JEBFVOLFMLUKLF-IFPLVEIFSA-N Astaxanthin Natural products CC(=C/C=C/C(=C/C=C/C1=C(C)C(=O)C(O)CC1(C)C)/C)C=CC=C(/C)C=CC=C(/C)C=CC2=C(C)C(=O)C(O)CC2(C)C JEBFVOLFMLUKLF-IFPLVEIFSA-N 0.000 title claims abstract description 97
- 235000013793 astaxanthin Nutrition 0.000 title claims abstract description 97
- MQZIGYBFDRPAKN-ZWAPEEGVSA-N astaxanthin Chemical compound C([C@H](O)C(=O)C=1C)C(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)C(=O)[C@@H](O)CC1(C)C MQZIGYBFDRPAKN-ZWAPEEGVSA-N 0.000 title claims abstract description 97
- 229940022405 astaxanthin Drugs 0.000 title claims abstract description 97
- 239000001168 astaxanthin Substances 0.000 title claims abstract description 97
- 239000003094 microcapsule Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000463 material Substances 0.000 claims abstract description 46
- 238000001035 drying Methods 0.000 claims abstract description 35
- 239000002775 capsule Substances 0.000 claims abstract description 28
- 238000000265 homogenisation Methods 0.000 claims abstract description 24
- 229920002683 Glycosaminoglycan Polymers 0.000 claims abstract description 14
- 229930006000 Sucrose Natural products 0.000 claims abstract description 10
- 229940080313 sodium starch Drugs 0.000 claims abstract description 10
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000005720 sucrose Substances 0.000 claims abstract description 10
- -1 sucrose ester Chemical class 0.000 claims abstract description 10
- 150000004676 glycans Chemical class 0.000 claims abstract description 9
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- 238000000034 method Methods 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 18
- 239000000839 emulsion Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 9
- HDLNSTQYXPTXMC-UHFFFAOYSA-N Astaxanthin-diacetat Natural products O=C1C(OC(=O)C)CC(C)(C)C(C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC=2C(CC(C(=O)C=2C)OC(C)=O)(C)C)=C1C HDLNSTQYXPTXMC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- 241000168517 Haematococcus lacustris Species 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002674 hyaluronan Polymers 0.000 claims description 3
- 229960003160 hyaluronic acid Drugs 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
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- 235000010384 tocopherol Nutrition 0.000 claims description 3
- 239000011732 tocopherol Substances 0.000 claims description 3
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 claims description 3
- SQDAZGGFXASXDW-UHFFFAOYSA-N 5-bromo-2-(trifluoromethoxy)pyridine Chemical compound FC(F)(F)OC1=CC=C(Br)C=N1 SQDAZGGFXASXDW-UHFFFAOYSA-N 0.000 claims description 2
- 229920001287 Chondroitin sulfate Polymers 0.000 claims description 2
- 241000239366 Euphausiacea Species 0.000 claims description 2
- 229940059329 chondroitin sulfate Drugs 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000000419 plant extract Substances 0.000 claims description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 2
- 235000013824 polyphenols Nutrition 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 3
- 235000013361 beverage Nutrition 0.000 abstract description 2
- 239000002537 cosmetic Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 44
- 239000012071 phase Substances 0.000 description 39
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 30
- 239000003208 petroleum Substances 0.000 description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
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- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 2
- 241000238557 Decapoda Species 0.000 description 2
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- 239000003963 antioxidant agent Substances 0.000 description 2
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- 229920000084 Gum arabic Polymers 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 229920002774 Maltodextrin Polymers 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 241000978776 Senegalia senegal Species 0.000 description 1
- GCSPRLPXTPMSTL-IBDNADADSA-N [(2s,3r,4s,5s,6r)-2-[(2s,3s,4s,5r)-3,4-dihydroxy-2,5-bis(hydroxymethyl)oxolan-2-yl]-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[C@@]1([C@]2(CO)[C@H]([C@H](O)[C@@H](CO)O2)O)O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GCSPRLPXTPMSTL-IBDNADADSA-N 0.000 description 1
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- 235000010489 acacia gum Nutrition 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/20—Animal feeding-stuffs from material of animal origin
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
-
- 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
-
- 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
- A23L29/035—Organic compounds containing oxygen 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
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
-
- 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
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Molecular Biology (AREA)
- Organic Chemistry (AREA)
- Zoology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mycology (AREA)
- Biomedical Technology (AREA)
- Biotechnology (AREA)
- Physiology (AREA)
- Animal Husbandry (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a natural astaxanthin water-soluble microcapsule and a preparation method thereof. The capsule wall material consists of glycosaminoglycan, polysaccharide, sodium starch succinate and sucrose ester. The oil phase comprises natural astaxanthin and a stabilizer. The preparation method of the microcapsule comprises the following steps: s1, preparing a water phase containing capsule wall materials and an oil phase containing astaxanthin; s2, dispersing the oil phase in the water phase through emulsification and homogenization; s3, drying the mixture by low-temperature vacuum spray drying to prepare the microcapsule of the invention. The preparation method provided by the invention has high embedding rate, can obviously improve the stability and water dispersion performance of the natural astaxanthin, can obviously improve the absorption rate of the natural astaxanthin, and can be applied to products such as food, beverage, cosmetics, skin care products, medicines and the like.
Description
Technical Field
The invention belongs to the technical field of biological substance preparation, and particularly relates to a natural freshwater shrimp water-soluble microcapsule and a preparation method thereof.
Background
Natural astaxanthin is the strongest antioxidant which is known at present and can be produced naturally, is used as a novel active factor in food, beverage, cosmetics and medicines, and has great market potential. Astaxanthin is widely present in animals and plants, but unprocessed natural astaxanthin exists mainly in the form of oil-soluble esterified astaxanthin, is insoluble in water, and serves as a strong antioxidant, and is easily oxidized and degraded to lose activity when stored under normal conditions. The microcapsule can wrap the active substance in a protective layer formed by wall materials, isolate the contact of the active substance and the external environment and protect the wrapped active substance; the microcapsule embedding can also convert liquid natural astaxanthin into solid, thereby being convenient for transportation and use; by selecting the wall material, the microcapsule embedding can also achieve the water dispersion of the astaxanthin. Therefore, the natural astaxanthin is prepared into the microcapsule, which is an ideal processing method.
The invention patent of Chinese patent No. 201210561599.7, which was applied at 12/22/2012, provides a method for preparing astaxanthin microcapsules, but the astaxanthin microcapsules produced by the method have large particles, poor water dispersibility, low astaxanthin embedding rate and poor stability of the formed microcapsules. The invention patent of Chinese patent No. 200810244049.6, applied on 19.12.2008, also discloses a preparation method of astaxanthin microcapsules, but the microcapsules produced by the method have low astaxanthin content and poor capsule stability. The chinese patent No. 201510152395.1, filed on 4/2/2015, provides another method for preparing astaxanthin microcapsules, which is slightly improved in capsule particle size and water dispersibility, but has problems of low encapsulation efficiency and poor microcapsule stability.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a natural freshwater shrimp water-soluble microcapsule formula and a preparation method thereof, and the specific technical scheme is as follows:
the invention provides a natural astaxanthin water-soluble microcapsule, which comprises a capsule wall material and an oil phase containing natural astaxanthin, wherein the oil phase is wrapped by the capsule wall material, and the capsule wall material comprises glycosaminoglycan, polysaccharide, sodium starch succinate and sucrose ester.
Preferably, the glycosaminoglycan is one or more of hyaluronic acid and chondroitin sulfate.
Preferably, the oil phase containing natural astaxanthin and wrapped by the capsule wall material comprises the following raw material components: natural astaxanthin and a stabilizer.
Preferably, the natural astaxanthin refers to an oil-soluble substance which is obtained from haematococcus pluvialis cells and krill and has no chemical processing, and the main component of the oil-soluble substance is astaxanthin ester;
the stabilizer is oil-soluble substance, and is one or more of plant extract, tocopherol and its derivatives, and natural polyphenol.
Preferably, the invention also provides a preparation method of the natural astaxanthin water-soluble microcapsule, which comprises the following steps:
s1, preparing a water phase containing capsule wall materials and an oil phase containing natural astaxanthin;
s2, dispersing an oil phase containing natural astaxanthin into a water phase containing capsule wall materials to prepare emulsion through emulsification and homogenization;
s3, drying the emulsion by low-temperature vacuum spray drying to prepare the microcapsule.
Preferably, the capsule wall material comprises glycosaminoglycan, polysaccharide, sodium starch succinate and sucrose ester, and the components of the capsule wall material are mixed with water and dissolved to form a water phase containing the capsule wall material, wherein the weight ratio of glycosaminoglycan to water is 1: 20-1: 3, the weight ratio of polysaccharide to water is 1: 20-1: 3, the weight ratio of sodium starch succinate to water is 1: 20-1: 3, and the weight ratio of sucrose ester to water is 1: 500-1: 100;
the oil phase containing the natural astaxanthin and wrapped by the capsule wall material comprises natural astaxanthin and a stabilizer, and the components of the oil phase containing the natural astaxanthin and wrapped by the capsule wall material are mixed and heated to 30-40 ℃ to be dissolved to prepare the oil phase containing the natural astaxanthin; wherein, the natural astaxanthin accounts for 90-99% of the total weight of the oil phase, and the stabilizer accounts for 1-10% of the total weight of the oil phase.
Preferably, step S2 specifically includes: mixing the water phase containing the capsule wall material and the oil phase containing the natural astaxanthin in the step S1, and emulsifying and homogenizing to prepare emulsion containing the natural astaxanthin, wherein the ratio of the water phase to the oil phase is 5: 1-1: 5;
the emulsification and homogenization method comprises high-speed homogenization and high-pressure homogenization, wherein the water phase and the oil phase are mixed and then are subjected to high-speed homogenization, and then are subjected to high-pressure homogenization; the rotation speed for high-speed homogenization is 14000-26000 rpm, and the high-speed homogenization time is O.5-10 minutes; the pressure used for high-pressure homogenization is 800-1500 bar, and the number of times of high-pressure homogenization is 1-20; the particle size of the emulsion prepared after high-pressure homogenization is 50-500 nm.
Preferably, step S3 specifically includes: drying the emulsion obtained in the step S2 to prepare microcapsules containing natural astaxanthin by low-temperature vacuum spray drying, wherein the drying gas used in the drying process is nitrogen;
the drying method comprises the steps of low-temperature vacuum spray drying, atomizing materials to be dried in a drying cavity, introducing drying gas, generating negative pressure in the drying cavity by using a vacuum pump to promote evaporation of water contained in the materials, and reducing the temperature of the required drying gas, wherein the particle size of the atomized materials is 1-100 microns, the vacuum degree in the drying cavity is-0.1-0.01 MPa, the air inlet temperature of the drying cavity is 30-40 ℃, and the air outlet temperature of the drying cavity is 20-30 ℃.
Preferably, the particle size of the oil phase containing astaxanthin dispersed in water is 100 to 900 nm.
Compared with the prior art, the invention has the following beneficial effects:
compared with the prior art, the method reduces the loss of natural astaxanthin in the production process of the microcapsule, improves the storage stability of the microcapsule, improves the embedding rate of an oil phase in the microcapsule and improves the water dispersion performance of the prepared microcapsule by reducing the temperature of the technological process, and comprises the following steps: the dissolving speed is improved, the particle size of an oil phase dispersed in water after dissolving and the stability after dissolving are reduced, and the absorption rate in oral administration and external application is improved.
Astaxanthin belongs to heat-sensitive substances and is easily degraded at higher temperature. The method of the invention utilizes negative pressure to reduce the boiling point of water by using low-temperature vacuum spray drying, and can quickly evaporate the moisture in the material on the premise of not raising the temperature of the drying gas, thereby completing the instant drying process which can be achieved by a common process only under high temperature. Therefore, the method obviously reduces the highest temperature used in the preparation process of the natural astaxanthin microcapsules, can finish drying at the temperature close to room temperature, avoids high temperature, simultaneously, uses nitrogen as the drying gas, completely avoids the oxidation of the astaxanthin in the processing process caused by using air as the drying gas, and has almost zero astaxanthin loss in the whole set of drying process which is far superior to the prior art.
According to the invention, glycosaminoglycan, polysaccharide, sodium starch succinate and sucrose ester are used as wall material raw materials, so that the use of animal derived gums, proteins and other substances is avoided, the production cost can be reduced, and meanwhile, compared with other wall material components, the wall material component used in the invention has better storage stability. The water solubility of the wall material is far better than that of the wall material used in the existing process, so that the dissolving speed of the microcapsule powder prepared by the method is greatly improved. The glycosaminoglycan is an inherently present component in the human body and thus has a higher absorption rate after entering the human body, and the absorption rate of the effective component astaxanthin in the microcapsules prepared according to the method of the present invention is significantly improved by using the glycosaminoglycan, compared to the microcapsules prepared by the existing techniques. In addition, by utilizing the synergistic effect of different components in the wall material, particularly glycosaminoglycan and sucrose ester, the emulsifying property of the wall material is greatly increased, and the particle size of the oil phase embedded in the microcapsule is obviously smaller than that of the existing similar products by matching high-speed and high-pressure homogenization, so that: 1) the embedding rate of the oil phase is improved, the oxidation of the oil phase and natural astaxanthin in the oil phase during the storage period is reduced, and the storage stability of the microcapsule is improved; 2) the particle size of the oil phase dispersed in water after water dissolution is obviously reduced, the clarity and physical stability after dissolution are improved, and the absorption utilization rate of the astaxanthin during oral administration and external use is improved.
In addition to the advantages, the invention uses glycosaminoglycan, polysaccharide, sodium starch succinate and sucrose ester as wall materials and is matched with low-temperature vacuum spray drying, and negative pressure is applied to the undried materials under the low-temperature condition by virtue of the characteristics of excellent molding and drying setting properties of the wall materials, so that the temperature required by drying is remarkably reduced, and meanwhile, the prepared microcapsule is in a porous structure on the premise of ensuring that an oil phase is completely wrapped by the wall materials, the ratio of the surface area to the volume of the microcapsule is effectively improved, and the dissolving speed of the microcapsule prepared by the method is further improved.
According to the scheme, the stabilizing agent is added into the oil phase, and the smaller oil phase particle size is matched, so that the microcapsule prepared by the method disclosed by the invention can keep physical and chemical stability for a long time after being dissolved in water. Therefore, the natural astaxanthin microcapsules prepared by the method can be used as powder or liquid after being dissolved in water, have a wider application range than the astaxanthin microcapsules prepared by the existing technology, and can be used in the application scenes of solid powder or liquid after being dissolved.
Detailed Description
The following examples are provided to illustrate the preparation of microcapsules of the present invention, and are intended to better illustrate the invention without limiting the composition and preparation of the microcapsules.
Example 1
Adding 3g tocopherol into 27g Haematococcus pluvialis extract containing 10% astaxanthin, and stirring at 40 deg.C to obtain oil phase. 0.5g sucrose laurate, 15g medium chain hyaluronic acid, 5g lactose, 10g resistant dextrin, 15g sodium starch succinate were dissolved in 100g water to form an aqueous phase.
Mixing the oil phase and the water phase, homogenizing at high speed with high speed shearing emulsifying machine (Wiggens, D-500, China) to obtain coarse emulsion (18000rpm, 5 min), and homogenizing at high pressure with high pressure homogenizer (ATS, AH-NANO, China) at 1000bar for 4 times to obtain emulsion with particle size of 190 nm.
The above emulsion was dried by vacuum low temperature spray (Yacheng, YC-2100, China) to prepare microcapsules, using nitrogen as the drying gas. The parameters of the spraying process are as follows: the air inlet temperature was 38 ℃, the air outlet temperature was 26 ℃, the atomization particle size was 5 μm, and the vacuum degree was-0.09 MPa, as in comparative example 1
27g of Haematococcus pluvialis extract having an astaxanthin content of 10% was used as the oil phase. 22g of gum arabic was dissolved with 23g of maltodextrin in 100g of water to form an aqueous phase.
Mixing the oil phase and the water phase, homogenizing at high speed with a high speed shearing emulsifying machine (Wiggens, D-500, China) to obtain emulsion (30000rpm, 5 min), with particle size of 810 nm.
The emulsion is spray dried (Yacheng, YC-1000, China; inlet air temperature 125 deg.C, outlet air temperature 83 deg.C, and atomization granularity 5um) to prepare microcapsule, and air is used as drying gas.
The following table shows the parameter comparison of the microcapsules obtained according to the process described in example 1 and comparative example 1:
the analytical detection method used in the examples of the present invention is as follows:
(1) particle size detection
The microcapsules prepared by the method of the invention are dissolved by pure water according to the weight ratio of 1: 25, and after the particles are completely dissolved, the particle size distribution is measured by using a light-dependent nano particle size distribution instrument (Jinan micro-nano, 802).
(2) Determination of astaxanthin content in natural astaxanthin ester
The natural astaxanthin ester is put into acetone according to the weight ratio of 1: 50. And after the astaxanthin ester is completely dissolved, taking the supernatant and filling the supernatant into a clean container. To the above acetone solution was added Tris-HCl pH7.0 buffer containing cholesterol esterase at a volume ratio of 1: 1, the concentration of cholesterol esterase in the buffer being 4 units/mL. The reaction was carried out at 37 ℃ for 45 minutes to convert the astaxanthin ester to free astaxanthin. Adding petroleum ether into the solution according to the volume ratio of 1: 1 to extract free astaxanthin into the petroleum ether. The aqueous phase of petroleum ether and also acetone was separated by centrifugation, and the petroleum ether was carefully removed and placed in a clean container. Petroleum ether was evaporated at low temperature using nitrogen and the dried residue was dissolved in high purity acetone in a volume ratio of 1: 1 to acetone diluent. 20 μ L of the above highly pure acetone solution was analyzed by high performance liquid chromatography (Agilent, Infinity 1260, USA; column Infinity Lab 120HILIC 2.1X150mm, 2.7 μm, Agilent, USA; mobile phase 82: 18 hexane: acetone; flow rate 1 mL/min; quantitative wavelength 474 nm). The final astaxanthin concentration was calculated from the astaxanthin standard curve (astaxanthin standard ≥ 98%, sigma, germany).
(3) Microcapsule astaxanthin content determination
Weighing 5mg of the microcapsules prepared by the method of the invention, placing the microcapsules in 1mL of acetone, crushing the microcapsules with a cell crusher (Osheng, Bioprep-24, China) (10 stainless steel balls with 2.8mm, 30 seconds, 6.5m/s, 9 cycles), centrifuging the microcapsules, taking out the supernatant, placing the supernatant into a clean container, extracting the precipitate with 1mL of acetone for 4 times, and collecting the supernatant after each extraction and centrifugation in the same container with the crushed and centrifuged supernatant. The acetone solution in this vessel was diluted 10-fold to obtain an acetone diluted solution. To the above acetone dilution was added Tris-HCl pH7.0 buffer containing cholesterol esterase at a concentration of 4 units/mL in the buffer at a volume ratio of 1: 1. The reaction was carried out at 37 ℃ for 45 minutes to convert the astaxanthin ester to free astaxanthin. Adding petroleum ether into the solution according to the volume ratio of 1: 1, and extracting free astaxanthin into the petroleum ether. The aqueous phase of petroleum ether and also acetone was separated by centrifugation, and the petroleum ether was carefully removed and placed in a clean container. Petroleum ether was evaporated at low temperature using nitrogen and the dried residue was dissolved in high purity acetone in a volume ratio of 1: 1 to acetone diluent. 20 μ L of the above highly pure acetone solution was analyzed by high performance liquid chromatography (Infinity 1260, Agilent, USA; column Infinity Lab 120HILIC 2.1X150mm, 2.7 μm, Agilent, USA; mobile phase 82: 18 hexane: acetone; flow rate 1 mL/min; quantitative wavelength 474 nm). The final astaxanthin concentration was calculated from the astaxanthin standard curve (astaxanthin standard ≥ 98%, sigma, germany). The encapsulation efficiency of the microcapsules was the astaxanthin content of the microcapsules divided by the astaxanthin content of the natural astaxanthin ester added when the same amount of microcapsules was prepared.
(4) Determination of astaxanthin content in serum
Centrifuging mouse blood, collecting supernatant to obtain serum, adding petroleum ether with volume ratio of 1: 1 into the serum, and extracting free astaxanthin into the petroleum ether. The petroleum ether and the aqueous phase containing acetone were separated by centrifugation, and the petroleum ether was carefully removed and placed in a clean container. Petroleum ether was evaporated at low temperature using nitrogen and the dried residue was dissolved in high purity acetone at a volume ratio of 1: 1 to acetone diluent. 20 μ L of the above highly pure acetone solution was analyzed by high performance liquid chromatography (Infinity 1260, Agilent, USA; column Infinity Lab 120HILIC 2.1X150mm, 2.7 μm, Agilent, USA; mobile phase 82: 18 hexane: acetone; flow rate 1 mL/min). The final astaxanthin concentration was calculated from the astaxanthin standard curve (astaxanthin standard ≥ 98%, sigma, germany).
(5) Oral administration experiment
Mice were fed with a feed containing 2g of astaxanthin microcapsules at a time, and blood was collected 1, 2, 4, and 8 hours after the feeding for analysis of the astaxanthin content in the serum.
(6) Experiment for external use
1g of astaxanthin microcapsules was dissolved in 10g of pure water, the obtained solution was applied to the back of a hairless mouse, the applied area was washed with pure water after 5 minutes, and then the absorbance of astaxanthin in the skin was analyzed by a spectrometer by using the absorption spectrum of astaxanthin.
It should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The water-soluble microcapsule of natural astaxanthin is characterized by comprising a capsule wall material and an oil phase containing the natural astaxanthin, wherein the oil phase is wrapped by the capsule wall material, and the capsule wall material comprises glycosaminoglycan, polysaccharide, sodium starch succinate and sucrose ester.
2. The water-soluble microcapsule of natural astaxanthin according to claim 1, wherein the glycosaminoglycan is one or more of hyaluronic acid and chondroitin sulfate.
3. The water-soluble microcapsule of natural astaxanthin according to claim 1, wherein the oil phase containing natural astaxanthin and wrapped by the capsule wall material comprises the following raw material components: natural astaxanthin and a stabilizer.
4. The natural astaxanthin water-soluble microcapsule according to claim 3, wherein the natural astaxanthin refers to an oil-soluble substance obtained from Haematococcus pluvialis cells, krill, and whose main chemically unprocessed component is astaxanthin ester;
the stabilizer is oil-soluble substance, and is one or more of plant extract, tocopherol and its derivatives, and natural polyphenol.
5. A method for preparing water-soluble microcapsules of natural astaxanthin according to any one of claims 1 to 4, comprising the following steps:
s1, preparing a water phase containing capsule wall materials and an oil phase containing natural astaxanthin;
s2, dispersing an oil phase containing natural astaxanthin into a water phase containing capsule wall materials to prepare emulsion through emulsification and homogenization;
s3, drying the emulsion through low-temperature vacuum spray drying to prepare the microcapsule.
6. The preparation method of the water-soluble microcapsule of natural astaxanthin according to claim 5, wherein the capsule wall material comprises glycosaminoglycan, polysaccharide, sodium starch succinate and sucrose ester, the components of the capsule wall material and water are mixed and dissolved to form a water phase containing the capsule wall material, wherein the weight ratio of glycosaminoglycan to water is 1: 20-1: 3, the weight ratio of polysaccharide to water is 1: 20-1: 3, the weight ratio of sodium starch succinate to water is 1: 20-1: 3, and the weight ratio of sucrose ester to water is 1: 500-1: 100;
the oil phase containing the natural astaxanthin and wrapped by the capsule wall material comprises natural astaxanthin and a stabilizer, and the components of the oil phase containing the natural astaxanthin and wrapped by the capsule wall material are mixed and heated to 30-40 ℃ to be dissolved to prepare the oil phase containing the natural astaxanthin; wherein, the natural astaxanthin accounts for 90-99% of the total weight of the oil phase, and the stabilizer accounts for 1-10% of the total weight of the oil phase.
7. The method for preparing water-soluble microcapsules of natural astaxanthin according to claim 5, wherein the step S2 specifically comprises: mixing the water phase containing the capsule wall material and the oil phase containing the natural astaxanthin in the step S1, and emulsifying and homogenizing to prepare the emulsion containing the natural astaxanthin, wherein the ratio of the water phase to the oil phase is 5: 1-1: 5;
the emulsification and homogenization method comprises high-speed homogenization and high-pressure homogenization, wherein the water phase and the oil phase are mixed and then are subjected to high-speed homogenization, and then are subjected to high-pressure homogenization; the rotation speed for high-speed homogenization is 14000-26000 rpm, and the high-speed homogenization time is 0.5-10 minutes; the pressure used for high-pressure homogenization is 800-1500 bar, and the number of times of high-pressure homogenization is 1-20; the particle size of the emulsion prepared after high-pressure homogenization is 50-500 nm.
8. The method for preparing water-soluble microcapsules of natural astaxanthin according to claim 5, wherein the step S3 specifically comprises: drying the emulsion obtained in the step S2 to prepare microcapsules containing natural astaxanthin by low-temperature vacuum spray drying, wherein the drying gas used in the drying process is nitrogen;
the drying method comprises the steps of low-temperature vacuum spray drying, atomizing materials to be dried in a drying cavity, introducing drying gas, generating negative pressure in the drying cavity by using a vacuum pump to promote evaporation of water contained in the materials, and reducing the temperature of the required drying gas, wherein the particle size of the atomized materials is 1-100 microns, the vacuum degree in the drying cavity is-0.1-0.01 MPa, the air inlet temperature of the drying cavity is 30-40 ℃, and the air outlet temperature of the drying cavity is 20-30 ℃.
9. The method for preparing a water-soluble microcapsule of natural astaxanthin according to claim 8, wherein the particle size of the oil phase containing astaxanthin dispersed in water is 100 to 900 nm.
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