CN110960492A - Astaxanthin freeze-dried powder and preparation method thereof - Google Patents

Astaxanthin freeze-dried powder and preparation method thereof Download PDF

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Publication number
CN110960492A
CN110960492A CN201911387174.7A CN201911387174A CN110960492A CN 110960492 A CN110960492 A CN 110960492A CN 201911387174 A CN201911387174 A CN 201911387174A CN 110960492 A CN110960492 A CN 110960492A
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astaxanthin
freeze
dried powder
ester
solution
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余建忠
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Fujian Qiyuantang Biotechnology Co ltd
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Fujian Qiyuantang Biotechnology Co ltd
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Abstract

The invention relates to the field of astaxanthin products, and relates to astaxanthin freeze-dried powder and a preparation method thereof, wherein the astaxanthin freeze-dried powder comprises astaxanthin ester, fatty glyceride, lecithin, chitosan, an emulsifier, a stabilizer, water and an excipient, and the addition amount of the chitosan is 1.2-1.5 times of the mass of the astaxanthin ester. The astaxanthin ester is dissolved by adopting the oil phase, the chitosan is added, the emulsion is formed by emulsification stabilization, and the freeze-dried powder is obtained by shaping, so that the astaxanthin utilization rate is high, and the activity retention degree is high.

Description

Astaxanthin freeze-dried powder and preparation method thereof
Technical Field
The invention relates to the field of astaxanthin products, and relates to astaxanthin freeze-dried powder and a preparation method thereof.
Background
Astaxanthin (English: Astaxanthin, also called Astaxanthin or Astaxanthin) is a kind of carotenoid, and is a strong natural antioxidant, and as with other carotenoids, Astaxanthin belongs to a fat-soluble and water-soluble pigment, and can be found in marine organisms such as shrimps, crabs, salmonids, algae, and the like, and has strong antioxidant capacity which is 550 times that of vitamin E and 10 times that of β -carotene.
Astaxanthin is added into products as an additive in the market at present. However, because astaxanthin is unstable and is easily decomposed by light, heat and high temperature, it is preferable that astaxanthin freeze-dried powder exists, for example, an astaxanthin freeze-dried powder and a preparation method thereof are disclosed in application publication No. CN110384632A in 2019, 10 and 29 months, and the formula of the astaxanthin freeze-dried powder comprises: 0.1-0.15% of astaxanthin, 5.96-8.78% of excipient and 91.47-94.22% of water phase. The preparation method comprises S11, adding the excipient into the water phase, and stirring at 200-500 r/min to dissolve completely to obtain a mixed solution; s12, uniformly stirring the mixed solution, filtering, sterilizing, and adding astaxanthin to obtain a mother solution; s13, freeze-drying the mother liquor to obtain freeze-dried powder.
The patent discloses astaxanthin freeze-dried powder for beauty treatment, which is obtained by mixing and freezing astaxanthin and excipient, while natural astaxanthin mainly exists in the form of astaxanthin ester, is an oil-soluble substance, has extremely poor water solubility, causes poor excipient effect and has great activity loss on astaxanthin.
Disclosure of Invention
The invention aims to provide astaxanthin freeze-dried powder, which overcomes the defects of the astaxanthin freeze-dried powder in the prior art.
The invention adopts the following technical scheme:
an astaxanthin freeze-dried powder comprises astaxanthin ester, fatty glyceride, lecithin, emulsifier, stabilizer, water, and excipient.
According to the technical scheme, the astaxanthin ester is dissolved by adopting the oil phase, emulsion is formed through emulsification stabilization, and freeze-dried powder is obtained through forming, so that the astaxanthin utilization rate is high, and the activity retention degree is high.
The combination of the fatty glyceride and the lecithin is adopted in the technical scheme, so that the emulsification and the forming of the astaxanthin are facilitated, the emulsification progress is accelerated, and the risk of astaxanthin decomposition is reduced.
Preferably, the ratio of each component in the astaxanthin freeze-dried powder is as follows:
1.5-6 parts of emulsion: astaxanthin ester, fatty glyceride, lecithin, emulsifier, stabilizer and water;
81-90 parts by weight of excipient.
More preferably, 2-4 parts by weight of the emulsion and 85-90 parts by weight of the excipient.
Wherein the mass volume ratio of astaxanthin ester to (sum of fatty glyceride and lecithin) is 0.18-0.25 g/ml.
Wherein the mixing ratio of the fatty glyceride to the lecithin is 3.6-4.5: 1.
Further preferably, the mixing ratio of the fatty acid glyceride and the lecithin is 4.0-4.5: 1.
Still more preferably, the mixing ratio of the fatty acid glyceride and the lecithin is 4.2: 1.
Preferably, chitosan is further added into the astaxanthin freeze-dried powder, so that the astaxanthin is favorably formed into micelles in a solution, the risk of decomposition is reduced, the activity of the astaxanthin can be kept to the maximum extent, and in addition, the addition of the chitosan is also favorably beneficial to the dispersion of the astaxanthin, so that the formed emulsion is uniform.
Preferably, the amount of chitosan added is 1.2 to 1.5 times the mass of the astaxanthin ester.
Preferably, the chitosan is added in the form of a chitosan solution.
Preferably, the mass concentration of the chitosan solution is 32-50%.
Preferably, the emulsifier is a polyglycerol ester.
The stabilizer is one or more of ascorbic acid or sodium salt thereof, ethylene diamine tetraacetic acid or sodium salt thereof and tea polyphenol, and the mass volume fraction of the stabilizer in the water phase is 0.0005-10%.
An emulsifying aid is also added, wherein the emulsifying aid is one or more of ethanol, 1, 2-propylene glycol, 1, 3-propylene glycol and glycerol; wherein the volume ratio of the emulsifier to the co-emulsifier is 1: 0.001-1.
In order to obtain better effect, an oil-soluble stabilizer is optionally added in the step 1); the oil-soluble stabilizer comprises one or more of tocopherol, coenzyme Q and gallate.
The astaxanthin ester from natural sources comprises resources such as antarctic krill, haematococcus pluvialis, prawns, crabs and the like.
Specifically, the natural astaxanthin ester refers to an oil-soluble substance obtained from Haematococcus cells or krill and containing astaxanthin ester as a main component without chemical processing.
Preferably, the excipient comprises one or more of glycerol, mannitol, trehalose.
The invention also provides a preparation method of the astaxanthin freeze-dried powder, which comprises the following steps:
1) mixing fatty glyceride and lecithin to obtain oil solution;
2) dissolving astaxanthin ester in an oil solution at the temperature of 20-55 ℃ to obtain an astaxanthin ester solution;
3) adding a chitosan solution into the astaxanthin ester solution obtained in the step 2), maintaining the temperature at 42-52 ℃, and keeping the temperature for more than 30 min;
4) adding an emulsifier and/or a co-emulsifier into the astaxanthin ester-chitosan solution prepared in the step 3) at the temperature of 55-60 ℃, adding a water phase containing a water-soluble stabilizer, and homogenizing until the system is uniform to obtain an emulsion;
5) adding an excipient into the astaxanthin emulsion obtained in the step 4), uniformly stirring, and freeze-drying to obtain astaxanthin freeze-dried powder.
The invention also provides application of the astaxanthin freeze-dried powder in products such as food, beverage, cosmetics, skin care products, medicines and the like.
By implementing the technical scheme, the invention has the following advantages: the astaxanthin freeze-dried powder has good stability and high astaxanthin activity retention degree and can be stored for a long time.
Detailed Description
The invention is further illustrated by the following examples; it should be noted that a person skilled in the art may make several improvements and optimizations without departing from the inventive concept, and these improvements and optimizations should also be considered within the scope of protection of the present invention.
The test materials and reagents used in the following were commercially available products unless otherwise specified, and astaxanthin ester (astaxanthin content 33.2% based on free astaxanthin) extracted from Haematococcus pluvialis was used.
Example 1
A preparation method of astaxanthin freeze-dried powder comprises the following steps:
1) mixing fatty glyceride, lecithin and tocopherol in a proportion of 3.6: 1: 1 mixing to prepare an oil solution;
2) dissolving 1kg of astaxanthin ester in 5.6L of oil solution at 40 ℃ to obtain astaxanthin ester solution;
3) adding 4.0L of chitosan solution with the mass concentration of 50% into the astaxanthin ester solution obtained in the step 2), maintaining the temperature at 42 ℃, and preserving the temperature for 30 min;
4) adding Tween 80 into the astaxanthin ester-chitosan solution prepared in the step 3) at the temperature of 60 ℃, adding a phosphate buffer solution with the pH value of 7.0 dissolved with ethylene diamine tetraacetic acid in advance, and homogenizing at a high speed until the system is uniform to obtain an emulsion;
5) adding 88kg of excipient mannitol into 4.5kg of the astaxanthin emulsion obtained in the step 4), uniformly stirring, and freeze-drying to obtain astaxanthin freeze-dried powder.
Example 2:
1) mixing fatty glyceride and lecithin according to a ratio of 4.5:1 to prepare an oil solution;
2) dissolving 1kg of astaxanthin ester extracted from Haematococcus cells in 5.6L of oil solution at 55 deg.C to obtain astaxanthin ester solution;
3) adding 4.0L of chitosan solution with the mass concentration of 32% into the astaxanthin ester solution obtained in the step 2), maintaining the temperature at 52 ℃, and keeping the temperature for more than 30 min;
4) adding polyglycerol ester into the astaxanthin ester-chitosan solution prepared in the step 3) at 55 ℃, adding a phosphate buffer solution with the pH value of 7.0 dissolved with ascorbic acid in advance, and homogenizing at high speed until the system is uniform to obtain an emulsion;
5) taking 1.5kg of the astaxanthin emulsion obtained in the step 4), adding 85kg of excipient mannitol, uniformly stirring, and freeze-drying to obtain astaxanthin freeze-dried powder.
Example 3:
1) mixing fatty glyceride and lecithin according to a ratio of 4.0:1 to prepare an oil solution;
2) dissolving 1kg of astaxanthin ester extracted from Haematococcus cells in 5.6L of oil solution at 20 deg.C to obtain astaxanthin ester solution;
3) adding 4.0L of chitosan solution with the mass concentration of 45% into the astaxanthin ester solution obtained in the step 2), maintaining the temperature at 50 ℃, and keeping the temperature for more than 30 min;
4) adding polyglycerol ester into the astaxanthin ester-chitosan solution prepared in the step 3) at the temperature of 58 ℃, adding phosphate buffer solution, and homogenizing at high speed until the system is uniform to obtain emulsion;
5) adding 90kg of excipient mannitol into 6kg of the astaxanthin emulsion obtained in the step 4), uniformly stirring, and freeze-drying to obtain astaxanthin freeze-dried powder.
Example 4:
1) mixing fatty glyceride, lecithin and coenzyme Q according to a ratio of 4.5:1:0.5 to prepare an oil solution;
2) dissolving 1kg of astaxanthin ester extracted from Haematococcus cells in 5.6L of oil solution at 35 deg.C to obtain astaxanthin ester solution;
3) adding 4.0L of chitosan solution with the mass concentration of 45% into the astaxanthin ester solution obtained in the step 2), maintaining the temperature at 42 ℃, and preserving the temperature for 40 min;
4) adding Tween 80 into the astaxanthin ester-chitosan solution prepared in the step 3) at the temperature of 55 ℃, adding a phosphate buffer solution with the pH value of 7.0 dissolved with ethylene diamine tetraacetic acid in advance, and homogenizing at a high speed until the system is uniform to obtain an emulsion;
5) adding 85kg of excipient glycerol into 5kg of astaxanthin emulsion obtained in the step 4), uniformly stirring, and freeze-drying to obtain astaxanthin freeze-dried powder.
Example 5:
1) mixing fatty glyceride, lecithin and gallate ester at a ratio of 3.8:1:0.5 to obtain oil solution;
2) dissolving 1kg of astaxanthin ester extracted from haematococcus pluvialis cells in 5.6L of oil solution at the temperature of 20-55 ℃ to obtain astaxanthin ester solution;
3) adding 4.0L of chitosan solution with the mass concentration of 46% into the astaxanthin ester solution obtained in the step 2), maintaining the temperature at 42 ℃, and keeping the temperature for 35 min;
4) adding Tween 80 into the astaxanthin ester-chitosan solution prepared in the step 3) at the temperature of 60 ℃, adding a phosphate buffer solution with the pH value of 7.0 dissolved with ethylene diamine tetraacetic acid in advance, and homogenizing at a high speed until the system is uniform to obtain an emulsion;
5) adding 85kg of excipient trehalose into 3kg of the astaxanthin emulsion obtained in the step 4), uniformly stirring, and freeze-drying to obtain astaxanthin freeze-dried powder.
Comparative example 1:
the difference from example 5 is that ethyl acetate is used to replace the mixed solution of fatty glyceride and lecithin, namely step 1) ethyl acetate and gallic acid ester are prepared into oil solution according to the ratio of 4.8: 0.5.
Comparative example 2:
the difference from example 5 is that no chitosan was added.
Comparative example 3:
the difference from example 5 is that the chitosan solution has a mass concentration of 15%.
Comparative example 4:
the difference from example 5 is that the chitosan solution has a mass concentration of 25%.
Comparative example 5:
the difference from example 5 is that the chitosan solution has a mass concentration of 55%.
Comparative example 6:
the difference from example 5 is that chitosan was added in an amount of 0.5 of the astaxanthin ester.
Comparative example 7:
the difference from example 5 is that chitosan was added in an amount of 0.8 of the astaxanthin ester.
Comparative example 7:
the difference from example 5 is that chitosan was added in an amount of 2.0 parts of the astaxanthin ester.
Comparative example 8:
the difference from example 5 is that step 3) is: 4.0L of chitosan solution with the mass concentration of 46 percent is added into the astaxanthin ester solution obtained in the step 2).
Comparative example 9:
the difference from example 5 is that in step 3) the temperature was maintained at 25 ℃.
Comparative example 10:
the difference from example 5 is that in step 3) the temperature was maintained at 60 ℃.
Because the step of freeze drying belongs to the conventional step and has little influence on the stability of the astaxanthin, the astaxanthin emulsion is directly detected and the stability of the astaxanthin emulsion is determined in the detection of the product, and the analysis and detection method specifically comprises the following steps:
1. astaxanthin ester content determination
Weighing a certain weight of sample, placing the sample in a volumetric flask, and then diluting the sample with dimethyl sulfoxide until the absorbance value is between 0.3 and 0.8. Measuring the absorbance value of the sample at the wavelength of 485nm by taking dimethyl sulfoxide as a blank control, and calculating the content of astaxanthin ester in the sample by using the following formula:
astaxanthin ester% (a485nm f)/(1908 m)
Note: in the formula, A485nm is the absorbance value of a sample to be detected under 485 nm; f is the dilution multiple; 1908 is extinction coefficient; and m is the weight (g) of the sample to be tested.
2. Stability determination
Storing the sample at room temperature in a dark place for 20 days, diluting the emulsion with a phosphate buffer solution with pH7.0 according to needs during determination until the absorbance value is 0.3-0.8, then determining the content of the astaxanthin ester in the sample, and finally calculating the loss rate of the astaxanthin ester in the storage process to evaluate the stability of the sample.
The loss ratio of astaxanthin ester is (Cn-C0)/C0,
wherein Cn is the astaxanthin ester content of the sample in the storage process; c0 is the astaxanthin ester content of the starting sample.
The results are given in the following table:
Figure DEST_PATH_IMAGE002
from the above measurement results, it is found that the stability of astaxanthin can be significantly improved and the degradation rate of astaxanthin can be reduced according to the embodiment of the present invention.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (10)

1. An astaxanthin freeze-dried powder is characterized by comprising astaxanthin ester, fatty glyceride, lecithin, an emulsifier, a stabilizer, water and an excipient.
2. The astaxanthin freeze-dried powder according to claim 1, wherein the ratio of each component in the astaxanthin freeze-dried powder is as follows:
1.5-6 parts of emulsion: astaxanthin ester, fatty glyceride, lecithin, emulsifier, stabilizer and water;
81-90 parts by weight of excipient.
3. An astaxanthin freeze-dried powder according to claim 2, characterized in that the mass-to-volume ratio of astaxanthin ester to the sum of fatty acid glyceride and lecithin is 0.18-0.25 g/ml.
4. An astaxanthin freeze-dried powder according to claim 3, characterized in that the mixing ratio of the fatty acid glyceride to the lecithin is 3.6-4.5: 1.
5. An astaxanthin freeze-dried powder according to claim 1,2, 3 or 4, wherein chitosan is further added into the astaxanthin freeze-dried powder.
6. An astaxanthin freeze-dried powder according to claim 5, characterized in that the addition amount of chitosan is 1.2-1.5 times of the mass of astaxanthin ester.
7. The astaxanthin freeze-dried powder according to claim 5, wherein the chitosan is added in the form of a chitosan solution, and the mass concentration of the chitosan solution is 32% -50%.
8. An astaxanthin freeze-dried powder according to claim 1, characterized in that an oil-soluble stabilizer is optionally added in the step 1); the oil-soluble stabilizer comprises one or more of tocopherol, coenzyme Q and gallate.
9. A preparation method of astaxanthin freeze-dried powder comprises the following steps:
1) mixing fatty glyceride and lecithin to obtain oil solution;
2) dissolving astaxanthin ester in an oil solution at the temperature of 20-55 ℃ to obtain an astaxanthin ester solution;
3) adding a chitosan solution into the astaxanthin ester solution obtained in the step 2), maintaining the temperature at 42-52 ℃, and keeping the temperature for more than 30 min;
4) adding an emulsifier and/or a co-emulsifier into the astaxanthin ester-chitosan solution prepared in the step 3) at the temperature of 55-60 ℃, adding a water phase containing a water-soluble stabilizer, and homogenizing until the system is uniform to obtain an emulsion;
5) adding an excipient into the astaxanthin emulsion obtained in the step 4), uniformly stirring, and freeze-drying to obtain astaxanthin freeze-dried powder.
10. The use of astaxanthin freeze-dried powder according to claim 1 in food, beverage, cosmetic, skin care product and pharmaceutical product.
CN201911387174.7A 2019-12-30 2019-12-30 Astaxanthin freeze-dried powder and preparation method thereof Pending CN110960492A (en)

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Citations (4)

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CN105902401A (en) * 2016-05-25 2016-08-31 中国海洋大学 Method for preparing H-polymer or J-polymer astaxanthin polymer nano dispersion system and application
WO2019066068A1 (en) * 2017-09-29 2019-04-04 富士フイルム株式会社 Oil-in-water type emulsified composition, and food and beverage containing same
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Publication number Priority date Publication date Assignee Title
CN104352434A (en) * 2014-11-20 2015-02-18 中国海洋大学 High-stability astaxanthin ester self-microemulsion and preparation method thereof
CN105902401A (en) * 2016-05-25 2016-08-31 中国海洋大学 Method for preparing H-polymer or J-polymer astaxanthin polymer nano dispersion system and application
WO2019066068A1 (en) * 2017-09-29 2019-04-04 富士フイルム株式会社 Oil-in-water type emulsified composition, and food and beverage containing same
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