CN109480285A - A kind of haematococcus pluvialis soft capsule - Google Patents

A kind of haematococcus pluvialis soft capsule Download PDF

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Publication number
CN109480285A
CN109480285A CN201811500495.9A CN201811500495A CN109480285A CN 109480285 A CN109480285 A CN 109480285A CN 201811500495 A CN201811500495 A CN 201811500495A CN 109480285 A CN109480285 A CN 109480285A
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Prior art keywords
astaxanthin
ethyl acetate
haematococcus pluvialis
parts
added
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CN201811500495.9A
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Inventor
皮小云
武金昆
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Lijiang Chenghai Lake Natural Spirulina Production Base Co Ltd
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Lijiang Chenghai Lake Natural Spirulina Production Base Co Ltd
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Priority to CN201811500495.9A priority Critical patent/CN109480285A/en
Publication of CN109480285A publication Critical patent/CN109480285A/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Mycology (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The present invention relates to field of health care food, the astaxanthin extracted more particularly to a kind of haematococcus pluvialis and its application, it is an object of that present invention to provide the extracting method of the astaxanthin of haematococcus pluvialis extraction and the haematococcus pluvialis soft capsule prepared with the astaxanthin of the preparation, the astaxanthin of this method preparation has the characteristics that recovery rate height and the column chromatographic purifying rate of recovery.A kind of astaxanthin that haematococcus pluvialis extracts, preparation method is in accordance with the following steps: after haematococcus pluvialis drying and crushing, isometric ethyl acetate is added and carries out cryogrinding, then the water of 8-10 times of quality is added, and cellulase and pectase ultrasonication 1-2min, heat preservation hydrolysis, it is centrifugated supernatant and precipitating, ethyl acetate is added in precipitating to extract, after the ethyl acetate of ethyl acetate and precipitating extraction in supernatant is mixed, freeze-dried, purifying, obtains astaxanthin oil.

Description

A kind of haematococcus pluvialis soft capsule
Technical field
The present invention relates to field of health care food, and in particular to a kind of haematococcus pluvialis soft capsule and Astaxanthin In Haematococcus Pluvialis Preparation method.
Background technique
Astaxanthin is a kind of pigment of carotenoids, entitled 3, the 3'- dihydroxy-beta carotene -4,4'- bis- of chemistry Ketone is naturally present in the biology such as algae, shrimp, crab and salmon.Natural astaxanthin is a kind of with the active class Hu of high anti-oxidation Radish element, there is the anti-lipid peroxidation of 10 times of beta carotene antioxidant effects and 550 times of vitamin Es to react special for it Property, it cannot be synthesized in animal body, but it is substance necessary to human body and animal life activity.Studies have shown that astaxanthin The immunity of organism can be enhanced, the rehabilitations such as cardiovascular disease, immune system, inflammation and nervus retrogression can be assisted, together When have the function of anti-aging and repair ultraviolet injury, can be widely applied to aquatic products and livestock-raising, food and cosmetics with And medicinal industry, there is huge market potential.
Haematococcus pluvialis is a kind of single celled eukaryotic green alga, is subordinate to Chlorophyta, volvocales, haematococcus section, haematococcus.By Largely astaxanthin can be accumulated in the algae and red is presented, therefore is named haematococcus.Astaxanthin can be largely accumulated under particular circumstances, Its content is up to the 1.5-4% of dry cell weight, and therefore, haematococcus pluvialis is to generally acknowledge the best life for natural astaxanthin exploitation Goods and materials source, it has also become the research hotspot of international natural astaxanthin industry.Haematococcus pluvialis soft capsule is logical as nutritional health food U.S. FDA approval has been crossed, the oxidative damage of LDL- cholesterol, protection skin can resist ultraviolet radiation damage effectively in pre- resistant to blood And alleviate age-related macular degeneration etc..It was eaten through Ministry of Public Health's approval haematococcus pluvialis as new resources in 2010 in China Product, therefore Haematococcus pluvialis production natural astaxanthin is developed with huge market potential.
At present in the method for Haematococcus pluvialis production natural astaxanthin, generally include grinding, broken wall, organic solvent extract and Purifying and etc..Currently, most common astaxanthin purification process is column chromatography, commonly by continuous silica gel medium pressure column, polyamides Amine column etc..Wherein, silicagel column will not have an impact astaxanthin, but the rate of recovery is low, generally be not higher than 70%.Extraction process High temperature oxygen ambient is then another key factor of astaxanthin loss.The method that current decompression extracts can reduce mentioning for astaxanthin Temperature is taken, guarantees the recovery rate and stability of astaxanthin, but temperature condition at least will also be controlled at 60 DEG C or so.
Summary of the invention
It is an object of that present invention to provide the extraction sides of the soft capsule of haematococcus pluvialis preparation and Astaxanthin In Haematococcus Pluvialis The astaxanthin of method, this method preparation has the characteristics that recovery rate height and the column chromatographic purifying rate of recovery.
The astaxanthin that a kind of haematococcus pluvialis extracts, preparation method in accordance with the following steps:
1) isometric ethyl acetate after haematococcus pluvialis drying and crushing, will be added and carries out cryogrinding, obtain mixture The water of 8-10 times of quality is added into mixture A, obtains mixture B by A,
2) cellulase 0.4-0.5% and pectase 0.2-0.3% is added by the quality of mixture B, keeps initial temperature Not higher than 5 DEG C, with the ultrasonication 1-2min of 300W, 22-25KHz, then temperature is controlled and hydrolyzes 5- in 37-40 DEG C of heat preservation 10min is centrifugated supernatant and precipitating, the whole stirring of step 2), mixing speed 500-1000r/min;
3) after supernatant stratification, liquid separation, vacuum distillation obtains the ethyl acetate A containing astaxanthin;
4) ethyl acetate is added in precipitating to extract, separates, obtains the ethyl acetate B containing astaxanthin;
5) after mixing ethyl acetate A and B containing astaxanthin, freeze-drying is chromatographed pure using continuous silica gel medium pressure column Change, obtains astaxanthin oil.
Further, the astaxanthin oil can be used for preparing haematococcus pluvialis soft capsule, raw materials used proportion by weight Are as follows: 100-120 parts of astaxanthin oil, 370-400 parts of safflower seed oil.
Further, the raw material of used soft capsule shell includes to measure in parts by mass: 100-120 parts of gelatin, glycerol 50-60 parts, 0.3-0.4 parts of titanium dioxide, 0.01 part of Brown Ferric Oxide, 100-120 parts of purified water
The invention has the following beneficial effects:
Haematococcus pluvialis soft capsule of the invention has effects that anti-oxidant, anti-aging, protection eyesight and cardiovascular and cerebrovascular.It adopts It uses astaxanthin oil and safflower seed oil as primary raw material, astaxanthin oil is protected using safflower seed oil, ensure that astaxanthin The activity of oil.
The present invention prepares the process of astaxanthin, and whole temperature is lower than 40 DEG C, and astaxanthin almost damage by non-oxidation in extraction process It loses.The ethyl acetate of the first step grinds the effect by preextraction astaxanthin, and during the ultrasonication of second step, prawn Green element is protected, the astaxanthin that preventing portion sub-dip goes out, and is destroyed in the localized hyperthermia that ultrasonic wave effect generates, by super After sonication and enzymatic treatment, using onestep extraction, 97% astaxanthin can be obtained.Also, purifying is using continuous middle pressure silicon Plastic column chromatography, purification process is nonnutritive to astaxanthin, ensure that the bioactivity of product astaxanthin.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way The present invention.
Embodiment 1
A kind of haematococcus pluvialis soft capsule, raw materials used proportion by weight are as follows: 120 parts of astaxanthin oil, safflower seed oil 370 Part, 120 parts of gelatin, 60 parts of glycerol, 0.3 part of titanium dioxide, 0.01 part of Brown Ferric Oxide, 120 parts of purified water.
Embodiment 2
A kind of haematococcus pluvialis soft capsule, raw materials used proportion by weight are as follows: 120 parts of astaxanthin oil, safflower seed oil 375 Part, 110 parts of gelatin, 50 parts of glycerol, 0.4 part of titanium dioxide, 0.01 part of Brown Ferric Oxide, 110 parts of purified water.
Embodiment 3
A kind of haematococcus pluvialis soft capsule, raw materials used proportion by weight are as follows: 100 parts of astaxanthin oil, safflower seed oil 380 Part, 100 parts of gelatin, 55 parts of glycerol, 0.4 part of titanium dioxide, 0.01 part of Brown Ferric Oxide, 100 parts of purified water.
Embodiment 4
A kind of haematococcus pluvialis soft capsule, raw materials used proportion by weight are as follows: 110 parts of astaxanthin oil, safflower seed oil 400 Part, 105 parts of gelatin, 55 parts of glycerol, 0.35 part of titanium dioxide, 0.01 part of Brown Ferric Oxide, 115 parts of purified water.
Embodiment 5
A kind of haematococcus pluvialis soft capsule, raw materials used proportion by weight are as follows: 115 parts of astaxanthin oil, safflower seed oil 385 Part, 110 parts of gelatin, 55 parts of glycerol, 0.32 part of titanium dioxide, 0.01 part of Brown Ferric Oxide, 110 parts of purified water.
Embodiment 6
A kind of haematococcus pluvialis soft capsule, raw materials used proportion by weight are as follows: 120 parts of astaxanthin oil, safflower seed oil 390 Part, 120 parts of gelatin, 60 parts of glycerol, 0.4 part of titanium dioxide, 0.01 part of Brown Ferric Oxide, 100 parts of purified water.
Embodiment 7
The astaxanthin that a kind of haematococcus pluvialis extracts, preparation method in accordance with the following steps:
1) isometric ethyl acetate after haematococcus pluvialis drying and crushing, will be added and carries out cryogrinding, obtain mixture The water of 8 times of quality is added into mixture A, obtains mixture B by A,
2) cellulase 0.4% and pectase 0.2% is added by the quality of mixture B, initial temperature is kept to be not higher than 5 DEG C, with the ultrasonication 1min of 300W, 22KHz, then temperature is controlled and hydrolyzes 8min, centrifuge separation in 37-40 DEG C of heat preservation Supernatant and precipitating, the whole stirring of step 2), mixing speed 500r/min;
3) after supernatant stratification, liquid separation, vacuum distillation obtains the ethyl acetate A containing astaxanthin;
4) ethyl acetate is added in precipitating to extract, separates, obtains the ethyl acetate B containing astaxanthin;
5) after mixing ethyl acetate A and B containing astaxanthin, freeze-drying is chromatographed pure using continuous silica gel medium pressure column Change, obtains astaxanthin oil.
Embodiment 8
The astaxanthin that a kind of haematococcus pluvialis extracts, preparation method in accordance with the following steps:
1) isometric ethyl acetate after haematococcus pluvialis drying and crushing, will be added and carries out cryogrinding, obtain mixture The water of 8 times of quality is added into mixture A, obtains mixture B by A,
2) cellulase 0.4% and pectase 0.3% is added by the quality of mixture B, initial temperature is kept to be not higher than 5 DEG C, with the ultrasonication 1min of 300W, 25KHz, then temperature is controlled and hydrolyzes 5min, centrifuge separation in 37-40 DEG C of heat preservation Supernatant and precipitating, the whole stirring of step 2), mixing speed 800r/min;
3) after supernatant stratification, liquid separation, vacuum distillation obtains the ethyl acetate A containing astaxanthin;
4) ethyl acetate is added in precipitating to extract, separates, obtains the ethyl acetate B containing astaxanthin;
5) after mixing ethyl acetate A and B containing astaxanthin, freeze-drying is chromatographed pure using continuous silica gel medium pressure column Change, obtains astaxanthin oil.
Embodiment 9
The astaxanthin that a kind of haematococcus pluvialis extracts, preparation method in accordance with the following steps:
1) isometric ethyl acetate after haematococcus pluvialis drying and crushing, will be added and carries out cryogrinding, obtain mixture The water of 10 times of quality is added into mixture A, obtains mixture B by A,
2) cellulase 0.5% and pectase 0.2% is added by the quality of mixture B, initial temperature is kept to be not higher than 5 DEG C, with the ultrasonication 1-2min of 300W, 22KHz, then temperature is controlled and hydrolyzes 5min, centrifugation point in 37-40 DEG C of heat preservation From supernatant and precipitating, the whole stirring of step 2), mixing speed 500r/min;
3) after supernatant stratification, liquid separation, vacuum distillation obtains the ethyl acetate A containing astaxanthin;
4) ethyl acetate is added in precipitating to extract, separates, obtains the ethyl acetate B containing astaxanthin;
5) after mixing ethyl acetate A and B containing astaxanthin, freeze-drying is chromatographed pure using continuous silica gel medium pressure column Change, obtains astaxanthin oil.
Embodiment 10
The astaxanthin that a kind of haematococcus pluvialis extracts, preparation method in accordance with the following steps:
1) isometric ethyl acetate after haematococcus pluvialis drying and crushing, will be added and carries out cryogrinding, obtain mixture The water of 8 times of quality is added into mixture A, obtains mixture B by A,
2) cellulase 0.4% and pectase 0.3% is added by the quality of mixture B, initial temperature is kept to be not higher than 5 DEG C, with the ultrasonication 1-2min of 300W, 23KHz, then temperature is controlled and hydrolyzes 10min, centrifugation point in 37-40 DEG C of heat preservation From supernatant and precipitating, the whole stirring of step 2), mixing speed 1000r/min;
3) after supernatant stratification, liquid separation, vacuum distillation obtains the ethyl acetate A containing astaxanthin;
4) ethyl acetate is added in precipitating to extract, separates, obtains the ethyl acetate B containing astaxanthin;
5) after mixing ethyl acetate A and B containing astaxanthin, freeze-drying is chromatographed pure using continuous silica gel medium pressure column Change, obtains astaxanthin oil.
It will be understood by those skilled in the art that above embodiments are only exemplary embodiments, without departing substantially from spirit of the invention In the case where range, a variety of variations can be carried out, replaced and changed.

Claims (3)

1. a kind of haematococcus pluvialis soft capsule, which is characterized in that content is made of the raw material of following proportion by weight:
100-120 parts of astaxanthin oil, 370-400 parts of safflower seed oil.
2. a kind of haematococcus pluvialis soft capsule according to claim 1, which is characterized in that the raw material of soft capsule shell includes pressing Mass parts meter: 100-120 parts of gelatin, 50-60 parts of glycerol, 0.3-0.4 parts of titanium dioxide, 0.01 part of Brown Ferric Oxide, purified water 100-120 parts.
3. a kind of haematococcus pluvialis soft capsule according to claim 1, which is characterized in that
The astaxanthin oil preparation method is in accordance with the following steps:
1) isometric ethyl acetate after haematococcus pluvialis drying and crushing, will be added and carries out cryogrinding, obtain mixture A, to The water of 8-10 times of quality is added in mixture A, obtains mixture B,
2) cellulase 0.4-0.5% and pectase 0.2-0.3% is added by the quality of mixture B, keeps initial temperature not high In 5 DEG C, with the ultrasonication 1-2min of 300W, 22-25KHz, then temperature is controlled and hydrolyzes 5- in 37-40 DEG C of heat preservation 10min is centrifugated supernatant and precipitating, the whole stirring of step 2), mixing speed 500-1000r/min;
3) after supernatant stratification, liquid separation, vacuum distillation obtains the ethyl acetate A containing astaxanthin;
4) ethyl acetate is added in precipitating to extract, separates, obtains the ethyl acetate B containing astaxanthin;
5) after mixing ethyl acetate A and B containing astaxanthin, freeze-drying using continuous silica gel medium pressure column chromatographic purifying, is obtained To astaxanthin oil.
CN201811500495.9A 2018-12-10 2018-12-10 A kind of haematococcus pluvialis soft capsule Pending CN109480285A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110713450A (en) * 2019-10-17 2020-01-21 福建启元堂生物技术有限公司 Astaxanthin extraction method based on haematococcus pluvialis
CN115299606A (en) * 2022-09-14 2022-11-08 云南龙布瑞生物科技有限公司 Method for separating and purifying endogenous pigment from fresh microalgae cells
CN117044940A (en) * 2023-07-17 2023-11-14 青岛南极维康生物科技有限公司 Krill oil haematococcus pluvialis and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101978975A (en) * 2010-11-16 2011-02-23 云南绿A生物工程有限公司 Haematococcus extract preparation, and preparation method and use thereof
CN103880726A (en) * 2014-03-14 2014-06-25 山东省农业科学院农产品研究所 Method for extracting astaxanthin in haematococcus pluvialis by adopting enzymolysis method and grinding method through organic solvent
CN106923334A (en) * 2016-12-22 2017-07-07 云南爱尔康生物技术有限公司 A kind of astaxanthin flexible glue capsule formula and preparation method thereof
CN107805215A (en) * 2017-10-18 2018-03-16 海南三元星生物科技股份有限公司 A kind of extracting method of astaxanthin
CN108902958A (en) * 2018-07-20 2018-11-30 深圳市博奥生物科技有限公司 A kind of astaxanthin soft capsule and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101978975A (en) * 2010-11-16 2011-02-23 云南绿A生物工程有限公司 Haematococcus extract preparation, and preparation method and use thereof
CN103880726A (en) * 2014-03-14 2014-06-25 山东省农业科学院农产品研究所 Method for extracting astaxanthin in haematococcus pluvialis by adopting enzymolysis method and grinding method through organic solvent
CN106923334A (en) * 2016-12-22 2017-07-07 云南爱尔康生物技术有限公司 A kind of astaxanthin flexible glue capsule formula and preparation method thereof
CN107805215A (en) * 2017-10-18 2018-03-16 海南三元星生物科技股份有限公司 A kind of extracting method of astaxanthin
CN108902958A (en) * 2018-07-20 2018-11-30 深圳市博奥生物科技有限公司 A kind of astaxanthin soft capsule and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110713450A (en) * 2019-10-17 2020-01-21 福建启元堂生物技术有限公司 Astaxanthin extraction method based on haematococcus pluvialis
CN115299606A (en) * 2022-09-14 2022-11-08 云南龙布瑞生物科技有限公司 Method for separating and purifying endogenous pigment from fresh microalgae cells
CN115299606B (en) * 2022-09-14 2024-02-02 云南龙布瑞生物科技有限公司 Method for separating and purifying endogenous pigment from fresh microalgae cells
CN117044940A (en) * 2023-07-17 2023-11-14 青岛南极维康生物科技有限公司 Krill oil haematococcus pluvialis and preparation method thereof
CN117044940B (en) * 2023-07-17 2024-05-28 青岛南极维康生物科技有限公司 Krill oil haematococcus pluvialis and preparation method thereof

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