CN117882860A - Astaxanthin composition and preparation method and application thereof - Google Patents
Astaxanthin composition and preparation method and application thereof Download PDFInfo
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- CN117882860A CN117882860A CN202311834370.0A CN202311834370A CN117882860A CN 117882860 A CN117882860 A CN 117882860A CN 202311834370 A CN202311834370 A CN 202311834370A CN 117882860 A CN117882860 A CN 117882860A
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- starch
- component
- astaxanthin
- amylase
- bacillus
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- 239000000203 mixture Substances 0.000 title claims abstract description 115
- 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 113
- 235000013793 astaxanthin Nutrition 0.000 title claims abstract description 113
- 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 113
- 229940022405 astaxanthin Drugs 0.000 title claims abstract description 113
- 239000001168 astaxanthin Substances 0.000 title claims abstract description 113
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 5
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- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
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- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
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- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 3
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Landscapes
- Medicinal Preparation (AREA)
Abstract
The invention discloses an astaxanthin composition, which comprises the following raw material components in percentage by weight: 20-95% of a component I and 1-30% of a component II; wherein the component I is an oligosaccharide mixture enriched after starch is subjected to enzymatic hydrolysis or microbial fermentation or a derivative modified by taking the oligosaccharide mixture as a substrate; the component II is astaxanthin. The composition is prepared by mixing astaxanthin from natural sources with starch hydrolysate, shearing, emulsifying, drying or not drying, has good water dispersibility, is heat-resistant, acid-base and light-emitting, has no abnormal flavor, and has high bioavailability. Greatly expands the application of astaxanthin raw materials in the fields of foods, medicines and cosmetics, and simultaneously has simple production process, is beneficial to industrialization, and has no organic reagent residue and no synthetic additive.
Description
Technical Field
The invention belongs to the technical field of astaxanthin, and particularly relates to an astaxanthin composition, a preparation method and application thereof.
Background
Starch is a high molecular carbohydrate, a polysaccharide consisting of a single type of sugar unit. The basic constituent unit of starch is alpha-D-glucopyranose, and the covalent polymer formed by removing water molecules from glucose and connecting the glucose together through glycosidic bonds is the starch molecule. Under certain conditions, oligosaccharides with different polymerization degrees can be obtained after specific enzymatic hydrolysis or microbial fermentation. Oligosaccharides are not destroyed by human stomach acid and are not decomposed by digestive enzymes. But it can be utilized by bacterial fermentation in the intestine to convert to short chain fatty acids and lactic acid.
Astaxanthin has super-strong antioxidant capacity which is 500 times that of vitamin E, and besides, it has the functions of improving immunity, resisting aging, preventing arteriosclerosis and related diseases, maintaining the health of eyes and central nervous system, repairing after exercise, relieving fatigue, etc. Has wide application prospect in the aspects of health care products, medicines, cosmetics, food additives, aquaculture and the like.
Astaxanthin is fat-soluble and there are great limitations in practical use. Once it is desired to use it in a liquid or solid system, such as a beverage or tablet, a large amount of carrier such as an emulsifier, stabilizer, dispersant is required to maintain stability of the system, conventional stabilizers such as ethyl acetate, mono-diglycerides, polyglycerol fatty acid esters, polyoxyethylene, sorbitan monolaurate, polyoxyethylene, sorbitan monopalmitate, sorbitan monostearate, sorbitan tristearate, sorbitan monooleate, and the like, due to its liposoluble dissolution characteristics. On the other hand, chelation of the additive also inhibits the digestive absorption of astaxanthin to some extent. Moreover, if used as a fat-soluble component alone, it is difficult to reach the action part to exert the effect due to the acid-base environment of the stomach and intestine, and the release is also affected.
Finally, the natural astaxanthin is extracted from algae, has special fishy smell of algae, and is greatly limited in development and application in products.
Therefore, the development of an astaxanthin product which can adapt to acid and alkali, is more stable, has low fishy smell and higher bioavailability is the key for solving the application.
Disclosure of Invention
Based on the above problems, an object of the present invention is to provide an astaxanthin composition, which has good water dispersibility, heat resistance, acid-base resistance, light irradiation resistance, no algae fishy smell and high bioavailability.
It is another object of the present invention to provide a process for preparing the composition.
It is a further object of the present invention to provide uses and methods of use of the composition.
The aim and the technical problems of the invention are realized by adopting the following technical proposal.
In one aspect, the invention provides an astaxanthin composition, which comprises the following raw material components in percentage by weight: 20-95% of component I and 1-30% of component II; wherein the component I is an oligosaccharide mixture enriched after starch is subjected to enzymatic hydrolysis or microbial fermentation or a derivative modified by taking the oligosaccharide mixture as a substrate; the component II is astaxanthin.
In a preferred embodiment of the invention, the astaxanthin composition is fully water-soluble and comprises at least 15% astaxanthin.
In a preferred embodiment of the present invention, the modification method comprises heat treatment, microwave treatment, ionizing radiation treatment, ultrasonic treatment, ball milling treatment, extrusion treatment, high-pressure treatment, etherification, esterification, oxidation, crosslinking.
In a preferred embodiment of the invention, the astaxanthin composition is in the form of a liquid, a powder, a granulate.
In a preferred embodiment of the invention, the preparation of component I is as follows: preparing starch into a solution with the concentration of 1-50%, adjusting the pH value of the solution to 4-9.0, adding or not adding amylase/inoculating or not inoculating microorganisms, reacting for 0.5-5h at the temperature of 25-60 ℃, after the reaction is finished, raising the temperature to 50-90 ℃, adjusting the pH value to 2-8.0, adding or not adding amylase, reacting for 2-12 h, and after the reaction is finished, carrying out conventional enzyme deactivation and filtering treatment to obtain the solution containing the component I.
In a preferred embodiment of the present invention, the starch is selected from one or more of corn starch, wheat starch, potato starch, pea starch, tapioca starch, mung bean starch, rice starch, sweet potato starch; the enzyme is one or more selected from alpha-amylase, beta-amylase, CGT glucosyltransferase and isoamylase; the microorganism is selected from one or more of bacillus, thermophilic bacillus, circular bacillus, bacillus macerans, alkali-resistant bacillus megaterium and escherichia coli.
In a preferred embodiment of the invention, the component II is astaxanthin of natural origin, including in shells derived from algae, fungi, phytoplankton or shrimp, crab, shellfish.
In a preferred embodiment of the invention, the composition further comprises a component III, wherein the component III is an acceptable auxiliary material or filler in foods, medicines and cosmetics.
In a preferred embodiment of the invention, the component III is selected from one or more of microcrystalline cellulose, sodium carboxymethylcellulose, sodium alginate, soluble starch, sorbitol, calcium sulphate, magnesium stearate, calcium phosphate.
In another aspect of the present invention, there is provided a method for preparing an astaxanthin composition, the method comprising the steps of:
S1: preparing starch into a solution with the concentration of 1-50%, adjusting the pH value of the solution to 4-9.0, adding or not adding amylase/inoculating or not inoculating microorganisms, reacting for 0.5-5h at the temperature of 25-60 ℃, after the reaction is finished, raising the temperature to 50-90 ℃, adjusting the pH value to 2-8.0, adding or not adding amylase, reacting for 2-12 hours, and after the reaction is finished, obtaining the solution containing the component I through the steps of conventional enzyme deactivation, filtration and the like;
S2: and (3) slowly adding the component II into the solution containing the component I obtained in the step (S1), and mechanically stirring for 1-12 h at normal temperature to obtain a mixed solution containing the component I and the component II.
S3: and (3) according to the concentration of the mixed solution obtained in the step (S2), adding or not adding the component III, and finally drying the mixed solution to obtain the astaxanthin composition.
In a preferred embodiment of the present invention, the starch is selected from one or more of corn starch, wheat starch, potato starch, pea starch, tapioca starch, mung bean starch, rice starch, sweet potato starch; the enzyme is one or more selected from alpha-amylase, beta-amylase, CGT glucosyltransferase and isoamylase; the microorganism is selected from one or more of bacillus, thermophilic bacillus, circular bacillus, bacillus macerans, alkali-resistant bacillus megaterium and escherichia coli.
The invention also provides an application of the astaxanthin composition or the astaxanthin composition prepared according to the preparation method in foods, medicines and cosmetics.
By means of the technical scheme, the invention has at least the following advantages:
1) The astaxanthin from natural sources is mostly extracted from algae, has special algae fishy smell, and the astaxanthin-containing composition has no algae fishy smell after the special treatment of the invention, thus greatly improving the palatability and increasing the application possibility in foods, medicines and cosmetics;
2) The astaxanthin is fat-soluble and difficult to dissolve in water, and the astaxanthin composition of the invention has good water solubility no matter in liquid or powder, can be conveniently applied in a liquid system, does not need to add synthetic additives such as stabilizing agents, emulsifying agents and the like, and is more green and safer;
3) The prior art for improving the water solubility of astaxanthin by wrapping adopts sodium alginate or other additives as wrapping materials, and only improves the physical properties, has no effect on bioavailability and even can influence the digestion and absorption in vivo; the method of the invention can improve the bioavailability of astaxanthin in the composition in vivo and is healthier while ensuring the improvement of physical properties.
The foregoing description is only an overview of the present invention, and is intended to provide a more thorough understanding of the present invention, and is to be accorded the full scope of the present invention.
Drawings
FIG. 1 shows the trend of the scavenging ability of the compositions prepared according to examples 1 to 5 and comparative example 1 before and after digestion;
FIG. 2 shows the trend of the DPPH radical scavenging ability of the compositions prepared according to examples 1 to 5 before and after digestion of comparative example 1.
Detailed Description
In order to make the technical means, the creation features, the achievement of the purposes and the effects of the present invention easy to understand, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides an astaxanthin composition, which has good palatability and no algae fishy smell; has better water dispersibility, heat resistance, acid-base and illumination stability, and higher bioavailability, and greatly widens the application scene of the astaxanthin. The invention also provides a preparation method of the astaxanthin composition, and the production process of the astaxanthin composition is simple and beneficial to industrialization, and no organic reagent residue or synthetic additive is used. In addition, the invention also provides application and an application method of the composition.
Astaxanthin has super-strong antioxidant capacity, and besides it has effects of enhancing immunity, resisting aging, preventing arteriosclerosis and related diseases, maintaining eye and central nervous system health, repairing after exercise, and relieving fatigue. However, astaxanthin of natural origin is generally derived from algae extraction and has a particular fishy smell. In addition, astaxanthin is fat-soluble and poorly soluble in water, so that flavor and solubility can bring about many impediments to product development during practical use.
The existing fishy smell masking method is unhealthy and green due to the fact that a large amount of sugar or high-power sweetener or essence is used. Many schemes for improving the solubility of astaxanthin are available, and most of the schemes use embedding treatment, sodium alginate or other coating materials, and the schemes are only improved from the physical properties, so that the schemes have no effect on bioavailability, and even the digestion and absorption of the astaxanthin in vivo can be influenced after part of the additive is chelated with the astaxanthin. Therefore, a more green, safe and healthy way is needed to improve the solubility of astaxanthin so as to increase the application range of astaxanthin in different product systems and exert the efficacy of astaxanthin.
In one aspect the present invention provides an astaxanthin composition, said composition comprising the following components:
Component I: the component I is an oligosaccharide mixture enriched after starch is subjected to enzymatic hydrolysis or microbial fermentation or a derivative modified by taking the oligosaccharide mixture as a substrate;
component II: the component II is astaxanthin of natural source;
Preferably, the starch comprises one or more of corn starch, wheat starch, potato starch, pea starch, tapioca starch, mung bean starch, rice starch, sweet potato starch.
Still preferably, the enzyme for preparing component I comprises one or more of alpha-amylase, beta-amylase, CGT glucosyltransferase, isoamylase; the microorganism comprises one or more of bacillus, thermophilic bacillus, bacillus circulans, bacillus macerans, alkali-resistant bacillus megaterium and escherichia coli; the modification method comprises heat treatment, microwave treatment, ionization radiation treatment, ultrasonic treatment, ball milling treatment, extrusion treatment, high-pressure treatment, etherification, esterification, oxidation and crosslinking.
In a specific embodiment, the component I is an oligosaccharide mixture obtained by subjecting a mixture of tapioca starch, rice starch and pea starch to alpha-amylase, CGT glucosyltransferase, beta-amylase enzymolysis or escherichia coli fermentation, and then performing the steps of normal enzyme deactivation, filtration and the like.
In a more specific embodiment, the component I is an oligosaccharide mixture obtained by subjecting a mixture of tapioca starch and rice starch to alpha-amylase, CGT glucosyltransferase, enzymolysis, normal enzyme deactivation, filtration and the like.
In a more specific embodiment, the astaxanthin composition comprises at least 70% of the oligosaccharide mixture or a physically or chemically modified derivative with the oligosaccharide mixture as a substrate.
Starch is a high molecular carbohydrate, a polysaccharide consisting of a single type of sugar unit. The basic constituent unit of starch is alpha-D-glucopyranose, and the covalent polymer formed by removing water molecules from glucose and connecting the glucose together through glycosidic bonds is the starch molecule. After starch hydrolysis or fermentation, the molecules are hydrolyzed to the dextrin and oligosaccharide range, the number of substrate molecules is increased, and the tail end groups are increased. The special spatial structure forms a spiral structure with hydrophobic cavities and hydrophilicity, so that the spiral structure can form inclusion compounds. Inclusion of the encapsulated molecules within the cavity or between helices may prevent loss of the guest molecule during processing and storage or mask undesirable flavors.
The general operation is that after starch is hydrolyzed or fermented by microorganism, the starch needs to be separated and purified to obtain the target compound with single molecule. The compound is then used as a downstream product. The authors have found by chance that the enriched oligosaccharide mixture after hydrolysis or microbial fermentation of starch has the ability to encapsulate specific molecules. Based on the finding, the derivative which takes the oligosaccharide mixture enriched by starch after hydrolysis or microbial fermentation as a substrate after physical or chemical modification has a good wrapping effect. The encapsulation can significantly improve the water-dispersing properties of the encapsulated molecules.
The component II is astaxanthin of natural origin.
In a specific embodiment, the source of component ii is in the shell of an animal such as algae, fungi, phytoplankton, shrimp, crab, shellfish, etc.
In a more specific embodiment, the source of component ii is algae, fungi, phytoplankton.
Astaxanthin in nature is derived from algae, bacteria and phytoplankton. It has been found that many kinds of algae such as Haematococcus pluvialis, chlorella, chlamydomonas, euglena, and Chlorella contain astaxanthin.
Haematococcus pluvialis is a single-cell organism, and can promote cell growth when a nitrogen source is sufficient in the culture process; in the absence of a nitrogen source, the cells are stimulated to produce and accumulate astaxanthin in vivo. The haematococcus pluvialis for producing astaxanthin has the characteristics of quick cell reproduction, simple culture and easy extraction, and is considered as a microalgae with good astaxanthin production prospect. The astaxanthin in the excellent haematococcus pluvialis algae in foreign countries generally accounts for more than 90 percent of the total carotenoid, the production quality is better, the astaxanthin exists in an esterified form and accounts for 60 to 80 percent of the total carotenoid, and a small amount of astaxanthin exists in a free form. However, haematococcus pluvialis has the disadvantages of relatively high growth conditions, long culture period, light irradiation, wall breaking, astaxanthin release and the like.
Chlorella belongs to Chlorella of Chlorophyta, and has the characteristics of easy culture, rapid growth, high temperature resistance, extreme pH, easy outdoor culture, etc. The synthesized astaxanthin has partial advantages of both rhodotorula rubra and haematococcus pluvialis, and can be rapidly synthesized under the dark condition by using organic matters such as glucose as a carbon source and energy, wherein the optimal growth temperature and the optimal astaxanthin synthesis temperature are both close to the room temperature at 24 ℃. The higher the carbon-nitrogen ratio, the more favorable the synthesis of astaxanthin. The astaxanthin is accumulated in a large amount in cytoplasm in an esterified state, so that higher cell concentration is relatively easy to achieve, and the growth and propagation and the accumulation of the astaxanthin can be synchronously carried out.
In addition, chlamydomonas, euglena, umbelliferae, etc. also contain a certain amount of astaxanthin.
In addition, the astaxanthin composition also comprises a component III, wherein the component III is an auxiliary material or a filler acceptable in foods, medicines and cosmetics.
These adjuvants or fillers are known in the art and have the effect of mainly ensuring the mixing uniformity and processing properties among the materials, but do not have any of the solubility change and fishy smell masking effects described in the present invention and do not adversely affect the flavor of the product.
In some specific embodiments, these excipients include one or more of microcrystalline cellulose, sodium carboxymethyl cellulose, sodium alginate, soluble starch, sorbitol, calcium sulfate, magnesium stearate, calcium phosphate.
Based on the above description, in a specific embodiment, the present invention provides an astaxanthin composition comprising about 10% to 95% of said oligosaccharide mixture or a physically or chemically modified derivative based on said oligosaccharide mixture, and about 1% to 50% of astaxanthin, the balance being supplemented by acceptable water-soluble adjuvants or fillers in said food, pharmaceutical product, said specific amounts being determined at the time of application of said astaxanthin composition.
In a more preferred embodiment, the present invention provides an astaxanthin composition comprising about 20% to 95% of said oligosaccharide mixture or a physically or chemically modified derivative with the oligosaccharide mixture as a substrate, and about 1% to 30% of astaxanthin, the balance being supplemented by water-soluble adjuvants or fillers acceptable in said food, pharmaceutical product, said specific amounts being determined at the time of application of said astaxanthin composition.
In yet another preferred embodiment, the composition is in the form of a liquid, powder, granule.
In another aspect, the present patent discloses a process for the preparation of the astaxanthin composition, comprising the steps of:
S1, weighing starch, preparing a solution with a certain concentration, adjusting the pH value of the solution, and then carrying out a first reaction under a proper temperature condition with or without amylase/inoculation or microorganism inoculation; after the reaction is finished, the temperature is increased, the pH value is adjusted, and amylase enzyme is added or not added for carrying out a second reaction; after the reaction is finished, the solution of the component I is obtained through the steps of conventional enzyme deactivation, filtration and the like;
S2, slowly adding the component II into the solution containing the component I obtained in the step S1, and mechanically stirring at normal temperature to obtain a mixed solution containing the component I and the component II;
S3, according to the concentration of the mixed solution obtained in the step S2, the component III is added or not added, and the required composition is obtained by spray drying, freeze drying and other modes.
In some specific embodiments, in step S1: the concentration of the starch solution is 1-60%, and the pH value is 2-9; the temperature of the first reaction is 10-60 ℃ and the time is 0.5-10 h; the temperature is increased to 20-90 ℃ after the first reaction, the pH value is adjusted to 2-8.0, and the second reaction time is 1-15 hours; in step S2: the mechanical stirring time is 1-15 h.
In some more preferred embodiments, in step S1: the concentration of the starch solution is 1-50%, and the pH value is 4-9; the temperature of the first reaction is 25-60 ℃ and the time is 0.5-5 h; the temperature is increased to 50-90 ℃ after the first reaction, the pH value is adjusted to 2-8.0, and the second reaction time is 2-12 hours; in step S2: the mechanical stirring time is 1-12 h.
In another aspect, the invention also provides the application of the astaxanthin-containing composition in foods, medicines and cosmetics.
In some embodiments, astaxanthin compositions are used to prepare liquid functional beverages, and stabilization of the system is ensured without the need for stabilizer emulsifiers.
The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
Example 1:
the present example provides an astaxanthin composition, the preparation method of which is as follows:
1. 80g of tapioca starch and 20g of rice starch are weighed and prepared into a 30% solution, the pH value of the solution is adjusted to 7.0, 0.2% of alpha-amylase is added, and the mixture is reacted for 60 minutes at 60 ℃. After the reaction, the temperature was raised to 90℃and the pH was adjusted to 6.0, and 0.1% of CGT glycosyltransferase CGTase N16 (which was filed by 11/13/2023 as a patent application by Nanj Cheng De, a biological technology Co., ltd.) was added and reacted for 5 hours. After the reaction is finished, the solution containing the component I is obtained through the conventional steps of enzyme deactivation and filtration.
2. Accurately weighing 15g of the component II of the astaxanthin from the natural source, slowly adding the component II into the solution containing the component I obtained in the step 1, and mechanically stirring the mixture at normal temperature for 5 hours to obtain a mixed solution containing the component I and the component II.
3. According to the concentration of the mixed solution obtained in the step 2, a solid of the astaxanthin-containing composition is obtained by freeze-drying, and the solid is crushed to obtain a powder of the astaxanthin-containing composition.
Example 2:
the present example provides an astaxanthin composition, the preparation method of which is as follows:
1. 50g of tapioca starch and 50g of rice starch are weighed and prepared into 40% solution, the pH value of the solution is adjusted to 7.0, 0.3% of alpha-amylase is added, and the mixture is reacted for 40 minutes at 60 ℃. After the reaction, the temperature was raised to 90℃and the pH was adjusted to 7.0, followed by the addition of 0.15% CGT glycosyltransferase CGTase N16, and the reaction was continued for 6 hours. After the reaction is finished, the solution of the component I is obtained through the conventional steps of enzyme deactivation and filtration.
2. And (3) accurately weighing 20g of the component II of the astaxanthin from the natural source, slowly adding the component II into the solution containing the component I obtained in the step (1), and mechanically stirring at normal temperature for 6 hours to obtain a mixed solution containing the component I and the component II.
3. And 3% of microcrystalline cellulose is added according to the concentration of the mixed solution obtained in the step 2, and the powder of the astaxanthin-containing composition is obtained by spray drying after uniform stirring.
Example 3:
the present example provides an astaxanthin composition, the preparation method of which is as follows:
1. 80g of tapioca starch and 20g of rice starch are weighed and prepared into 50% solution, the pH value of the solution is adjusted to 6.0, 0.4% of alpha-amylase is added, and the mixture is reacted for 60 minutes at 60 ℃. After the reaction, the temperature was raised to 95℃and the pH was adjusted to 7.0, followed by the addition of 0.2% CGT glycosyltransferase CGTase N16, and the reaction was continued for 5 hours. After the reaction is finished, the solution of the component I is obtained through the conventional steps of enzyme deactivation and filtration.
2. Accurately weighing 30g of a component II of astaxanthin from natural sources, slowly adding the component II into the solution containing the component I obtained in the step 1, and mechanically stirring the solution at normal temperature for 10 hours to obtain a mixed solution containing the component I and the component II.
3. According to the concentration of the mixed solution obtained in the step 2, a solid of the astaxanthin-containing composition is obtained by freeze-drying, and the solid is crushed to obtain a powder of the astaxanthin-containing composition.
Example 4:
the present example provides an astaxanthin composition, the preparation method of which is as follows:
1. 20g of tapioca starch and 80g of rice starch are weighed and prepared into a 30% solution, the pH value of the solution is adjusted to 7.0, 0.2% of alpha-amylase is added, and the mixture is reacted for 30 minutes at 60 ℃. After the reaction, the temperature was raised to 90℃and the pH was adjusted to 8.0, followed by the addition of 0.2% CGT glycosyltransferase CGTase N16, and the reaction was continued for 6 hours. After the reaction is finished, the solution of the component I is obtained through the conventional steps of enzyme deactivation and filtration.
2. And (3) accurately weighing 18g of the component II of the astaxanthin from the natural source, slowly adding the component II into the solution containing the component I obtained in the step (1), and mechanically stirring at normal temperature for 7 hours to obtain a mixed solution containing the component I and the component II.
3. And (2) adding 2% of soluble starch according to the concentration of the mixed solution obtained in the step (2), uniformly stirring, and then obtaining the astaxanthin-containing composition powder by using a spray drying mode.
Example 5:
the present example provides an astaxanthin composition, the preparation method of which is as follows:
1. 30g of tapioca starch and 70g of rice starch are weighed and prepared into 40% solution, the pH value of the solution is adjusted to 7.0, 0.25% of alpha-amylase is added, and the mixture is reacted for 30 minutes at 60 ℃. After the reaction, the temperature was raised to 90℃and the pH was adjusted to 8.0, followed by the addition of 0.3% CGT glycosyltransferase CGTase N16, and the reaction was continued for 6 hours. After the reaction is finished, the solution of the component I is obtained through the conventional steps of enzyme deactivation and filtration.
2. Accurately weighing 25g of the component II of the astaxanthin from the natural source, slowly adding the component II into the solution containing the component I obtained in the step 1, and mechanically stirring the solution at normal temperature for 10 hours to obtain a mixed solution containing the component I and the component II.
3. According to the concentration of the mixed solution obtained in the step 2, 1% of soluble starch and 1% of microcrystalline cellulose are added, and the mixture is stirred uniformly and then subjected to spray drying to obtain the astaxanthin-containing composition powder.
Comparative example 1:
Comparative example 1 is a commercial astaxanthin-containing microcapsule powder (AM 20111601 content 10%) purportedly derived from natural haematococcus pluvialis.
Comparative example 2:
Comparative example 2 is a treatment without adding CGT glucosyltransferase CGTase N16 on the basis of example 1. The specific steps are 1, 80g of tapioca starch and 20g of rice starch are weighed and prepared into 30% solution, the pH value of the solution is regulated to 7.0, 0.2% of alpha-amylase is added, and the reaction is carried out for 60 minutes at the temperature of 60 ℃. After the reaction is finished, the solution containing the component I is obtained through the conventional steps of enzyme deactivation and filtration. 2. Accurately weighing 15g of the component II of the astaxanthin from the natural source, slowly adding the component II into the solution containing the component I obtained in the step 1, and mechanically stirring the mixture at normal temperature for 5 hours to obtain a mixed solution containing the component I and the component II.
3. According to the concentration of the mixed solution obtained in the step 2, a solid of the astaxanthin-containing composition is obtained by freeze-drying, and the solid is crushed to obtain a powder of the astaxanthin-containing composition.
Test example 1: comparison of flavors of different compositions
Liquid beverage 1 was prepared from astaxanthin in examples 3, 4,5 and comparative example 1, respectively, with the following formulation shown in table 1, and liquid beverage 2 was prepared from the compositions of example 1 and comparative examples 1 and 2, with the formulation shown in table 2:
table 1 liquid beverage 1 formulations of different examples
Table 2 liquid beverage 2 formulations of different examples
| Raw materials | Comparative example 1 | Comparative example 2 | Example 1 |
| Isomalt | 2 | 2 | 2 |
| Sodium hyaluronate | 0.15 | 0.15 | 0.15 |
| DL-malic acid | 0.1 | 0.1 | 0.1 |
| Citric acid | 0.05 | 0.05 | 0.05 |
| Ascorbic acid | 0.1 | 0.1 | 0.1 |
| Astaxanthin composition | 0.7 | 0.7 | 0.7 |
| Sodium carboxymethyl cellulose | 0.1 | 0.1 | 0.1 |
| Water and its preparation method | 96.8 | 96.8 | 96.8 |
Sensory evaluation was performed in the beverage formulation 1 of table 1 described above to ensure that the amounts of astaxanthin actually contained in each sample were the same and in the beverage formulation 2 of table 2 to ensure that the amounts of astaxanthin added were the same (sensory evaluation table is shown in table 3 below). The results of the evaluation for the beverage formulations of Table 1 are shown in Table 4 and the results of the evaluation for the beverage formulations of Table 2 are shown in Table 5. From the sensory evaluation results tables 4 and 5, it was found that astaxanthin-containing beverages prepared using the raw materials of examples 1, 2,3, 4, 5 had no fishy smell, no foreign smell, and good flavor as compared with comparative examples 1, 2. Illustrating that the compositions of examples 1, 2,3, 4, 5 prepared using the process of the present invention are effective in masking the fishy smell of astaxanthin.
Table 3 sensory evaluation table
Table 4 results of sensory evaluation of the beverage formulations of table 1
| Experimental group | Sensory score |
| Comparative example 1 | 68 |
| Comparative example 2 | 76 |
| Example 1 | 95 |
| Example 2 | 93 |
| Example 3 | 94 |
| Example 4 | 93 |
| Example 5 | 91 |
Table 5 results of sensory evaluation of the beverage formulations of table 2
| Experimental group | Sensory score |
| Comparative example 1 | 70 |
| Comparative example 2 | 74 |
| Example 1 | 94 |
Test example 2: stability comparison of different astaxanthin compositions
The compositions prepared in examples 1 to 5 and comparative examples 1 and 2 were subjected to accelerated experiments at 40℃and 75% humidity, and after leaving for 6 months, the astaxanthin content was measured at intervals of 1, 2, 3, 6 months, and the residual percentage was measured as compared with the original content. (content test method reference "GB/T31520-2015 determination of astaxanthin in Haematococcus liquid chromatography", residual Rate= (original content-test point content)/original content%).
The results are shown in Table 6.
TABLE 6 statistics of astaxanthin survival rate for different compositions
| Comparative example 1 | Comparative example 2 | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| 0 Month | 10％ | 8％ | 15％ | 20％ | 30％ | 18％ | 25％ |
| 1 Month | 9.80％ | 7.4％ | 14.80％ | 19.80％ | 29.90％ | 17.40％ | 24.60％ |
| 2 Months of | 9.20％ | 6.9％ | 14.40％ | 19.20％ | 29.60％ | 17.20％ | 24.50％ |
| 3 Months of | 8.50％ | 6.4％ | 14.20％ | 18.60％ | 29.20％ | 16.80％ | 24.10％ |
| 6 Months of | 7％ | 6％ | 13.80％ | 18.60％ | 28.90％ | 16.70％ | 23.90％ |
| Survival rate | 70.0％ | 60％ | 92.0％ | 93.0％ | 96.3％ | 92.8％ | 95.6％ |
From the analysis of the experimental results in Table 6, the astaxanthin compositions prepared in examples 1-5 showed significantly higher astaxanthin residual rate than comparative examples 1 and 2 under the condition of accelerating for 6 months, which indicated that the astaxanthin compositions prepared in accordance with the present invention had a more stable shelf life and a better stability.
Test example 3: in vitro digestion simulation
Simulation of the effect of gastrointestinal fluids on stability of the composition: the compositions of examples 1 to 5 and comparative examples 1 and 2 were prepared as 10% by mass solutions, simulated gastric fluid was added to each of the solutions, the simulated intestinal fluid was treated for 2 hours, and the pH of the simulated gastric fluid set was adjusted back to 6.9 to 7.3 to compare the changes in the ability to scavenge hydroxyl radicals and DPPH.radical, and the activities of the different compositions after digestion in simulated gastric fluid and simulated intestinal fluid were determined. Wherein the determination of the scavenging ability of hydroxyl radicals (HO. Cndot.) is wrong with the reference to the oxidation method of phenanthrene-Fe 2+, and the determination of the scavenging efficiency of DPPH. Cndot. Radical is performed by adopting a conventional spectrophotometry.
FIGS. 1 to 2 show the trend of the scavenging ability of comparative examples 1 to 2 and examples 1 to 5 against HO and DPPH radicals after simulated gastric fluid and intestinal fluid digestion. The results according to fig. 1-2 show that the compositions of examples 1-5 of the present invention still have higher bioactivity after gastrointestinal digestion and perform normal functions as compared with the compositions of comparative examples 1 and 2, as demonstrated by simulated gastric fluid and intestinal fluid tests. The astaxanthin composition prepared by the preparation method disclosed by the invention has relatively stable temperature and acid-base tolerance, and can obviously reduce the influence of processing conditions on active ingredients of the composition.
The present invention is not described in detail in the present application, and is well known to those skilled in the art.
While the invention has been described with respect to preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and that any such changes and modifications as described in the above embodiments are intended to be within the scope of the invention.
Claims (10)
1. An astaxanthin composition, which is characterized by comprising the following raw material components in percentage by weight: 20-95% of a component I and 1-30% of a component II; wherein the component I is an oligosaccharide mixture enriched after starch is subjected to enzymatic hydrolysis or microbial fermentation or a derivative modified by taking the oligosaccharide mixture as a substrate; the component II is astaxanthin.
2. The composition according to claim 1, wherein the preparation process of component I is: preparing starch into a solution with the concentration of 1-50%, adjusting the pH value of the solution to 4-9.0, adding or not adding amylase/inoculating or not inoculating microorganisms, reacting for 0.5-5h at the temperature of 25-60 ℃, after the reaction is finished, raising the temperature to 50-90 ℃, adjusting the pH value to 2-8.0, adding or not adding amylase, reacting for 2-12 h, and after the reaction is finished, carrying out conventional enzyme deactivation and filtering treatment to obtain the solution containing the component I.
3. The composition according to claim 1 or 2, wherein the starch is selected from one or more of corn starch, wheat starch, potato starch, pea starch, tapioca starch, mung bean starch, rice starch, sweet potato starch; the enzyme is one or more selected from alpha-amylase, beta-amylase, CGT glucosyltransferase and isoamylase; the microorganism is selected from one or more of bacillus, thermophilic bacillus, circular bacillus, bacillus macerans, alkali-resistant bacillus megaterium and escherichia coli.
4. The composition according to claim 1, wherein the component ii is an astaxanthin of natural origin, including in shells derived from algae, fungi, phytoplankton or shrimp, crab, shellfish.
5. The composition of claim 1, further comprising component III, wherein component III is a food, pharmaceutical, cosmetic acceptable adjuvant or filler.
6. The composition according to claim 6, wherein component III is selected from one or more of microcrystalline cellulose, sodium carboxymethyl cellulose, sodium alginate, soluble starch, sorbitol, calcium sulfate, magnesium stearate, calcium phosphate.
7. A process for the preparation of an astaxanthin composition according to any one of claims 1-7, said process comprising the steps of:
S1: preparing starch into a solution with the concentration of 1-50%, adjusting the pH value of the solution to 4-9.0, adding or not adding amylase/inoculating or not inoculating microorganisms, reacting for 0.5-5h at the temperature of 25-60 ℃, after the reaction is finished, raising the temperature to 50-90 ℃, adjusting the pH value to 2-8.0, adding or not adding amylase, reacting for 2-12 h, and after the reaction is finished, carrying out the steps of conventional enzyme deactivation, filtration and the like to obtain a solution containing the component I;
s2: and (3) slowly adding the component II into the solution containing the component I obtained in the step (S1), and mechanically stirring for 1-12 hours at normal temperature to obtain a mixed solution containing the component I and the component II.
S3: and (3) according to the concentration of the mixed solution obtained in the step (S2), adding or not adding the component III, and finally drying the mixed solution to obtain the astaxanthin composition.
9. The preparation method according to claim 8, wherein the starch is one or more selected from corn starch, wheat starch, potato starch, pea starch, tapioca starch, mung bean starch, rice starch, sweet potato starch; the enzyme is one or more selected from alpha-amylase, beta-amylase, CGT glucosyltransferase and isoamylase; the microorganism is selected from one or more of bacillus, thermophilic bacillus, circular bacillus, bacillus macerans, alkali-resistant bacillus megaterium and escherichia coli.
10. Use of an astaxanthin composition according to any one of claims 1-7 or prepared according to the preparation method of claim 8 or 9 in food, pharmaceutical, cosmetic.
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| CN202311834370.0A CN117882860A (en) | 2023-12-28 | 2023-12-28 | Astaxanthin composition and preparation method and application thereof |
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