CN102731359B - Extraction method of astaxanthin and ester thereof from antarctic krill - Google Patents

Extraction method of astaxanthin and ester thereof from antarctic krill Download PDF

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Publication number
CN102731359B
CN102731359B CN201210249101.3A CN201210249101A CN102731359B CN 102731359 B CN102731359 B CN 102731359B CN 201210249101 A CN201210249101 A CN 201210249101A CN 102731359 B CN102731359 B CN 102731359B
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ethanol
add
astaxanthin
red
stir
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CN102731359A (en
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刘代成
张倩
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Shandong Normal University
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Shandong Normal University
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Abstract

The invention discloses an extraction method of astaxanthin and ester thereof from antarctic krill. The method comprises the following steps: based on frozen antarctic krill as a raw material, extracting with ethanol; concentrating filtered extract, and adding chitin acetate solution; stirring, adsorbing and standing to obtain an upper red float; separating the float, and adding ethanol for stirring and eluting; filtering to obtain red ethanol eluate and white precipitate; removing ethanol to obtain the red paste, namely the astaxanthin and ester thereof; and stirring and dissolving the white precipitate with acetic acid, and filtering for recycling. According to the extraction method of the astaxanthin and ester thereof from antarctic krill, the frozen antarctic krill is used as the raw material, ethanol is used for extracting, and the process is simple; ethanol is still used in the process of preparing and eluting the astaxanthin and ester thereof from the red float, and the single solvent without toxicity is used in the whole process, so that the production process for recycling the solvent is easy, and the chitin can be recycled.

Description

A kind of method of extracting astaxanthin and ester thereof from krill
Technical field
The present invention relates to a kind of method of extracting astaxanthin and ester thereof from krill.
Background technology
Krill (Euphausia superba), has another name called large krill or krill, is the krill of one way of life in the waters, the Antarctica of Antarctic Ocean.Live in the mode of trooping, density reaches 10,000~30,000/m sometimes 3.They may be the most successful animal species on the earth, hundred million tons of nearly 5-50 (because methods of evaluation difference has larger difference).Annual approximately 100,000 tons of krill fishery.Mainly fishery country is Japan and Polish.Mainly be used as cooking in Japan, world's elsewhere is as animal-feed and bait.
Natural astaxanthin more than 90% exists with esterified form, more stable.Preparation, storage and the application of large multi-product are all carried out with the form of astaxanthin ester.Krill contains the astaxanthin ester that astaxanthin and astaxanthin are combined with lipid acid, astaxanthin and astaxanthin ester are applied in aquaculture, entering after animal body can be not modified or biochemical conversion and being directly stored in tissue, make skin and the muscle of some hydrocoles occur health and chromatic colour, make feather, skin, pin, the beak of birds, beasts and eggs and fowl present healthy golden yellow and red, be used as at present painted for food of foodstuff additive, fresh-keeping and nutrition.
Astaxanthin is a kind of good antioxidant, aspect the generation of antioxidant cancellation free radical, is playing an important role, and the resistance of oxidation of astaxanthin is than β-carotene and V emuch higher times.
Astaxanthin has the effect that promotes growth and breeding, can promote the Reproduction of fish, promotes fish-egg fertilization, reduces the mortality ratio of fetal development, accelerates individual growth, increases ripe speed and fecundity, can also improve the laying rate of poultry.
Astaxanthin has the effect that promotes growth and breeding, can promote the Reproduction of fish, promotes fish-egg fertilization, reduces the mortality ratio of fetal development, accelerates individual growth, increases ripe speed and fecundity, can also improve the laying rate of poultry.
Astaxanthin can effectively prevent by hemato encephalic barrier the damage of amphiblestroid oxidation and photoreceptor cell, can be used for prevention and treatment age-related macular degeneration, improves retinal function.Astaxanthin also have neuroprotective system especially brain and spinal cord be subject to effect of oxidative damage, can effectively treat the central nervous system diseases such as ischemic repetition perfusion injury, Spinal injury, parkinsonism, senile dementia.
Along with progressively going deep into of astaxanthin biological functional study and pharmacological effect test, astaxanthin is widely used in medicine, makeup and high-grade nutrient health care food industries.In makeup, add astaxanthin and can play anti-ageing, sun-proof texts, can keep for a long time painted and be beneficial to skin health for lipstick.
Raw material prepared by astaxanthin has shrimp, crab, shrimp shell, shrimp protein etc., and the hugest with krill resource, and astaxanthin and ester content thereof are abundant, are also the highest compositions of added value in krill shrimp sauce.Being separated by the simplest method, is one of technology of being badly in need of most on producing.
Summary of the invention
For above-mentioned prior art, the invention provides a kind of method of utilizing chitin to adsorb astaxanthin and ester thereof from krill extracting solution.
The present invention is achieved through the following technical solutions:
A method of extracting astaxanthin and ester thereof from krill, step is as follows:
(1) get the freezing fresh krill of 1 kilogram, add 1.0~1.4 liter of 95~100% ethanol (volume fraction), more than stirring extraction 3h, after leaving standstill, pour out extracting solution, 95~100% ethanol of the extracting solution equivalent adding again and pour out repeat to extract twice, extract altogether 3 times, extracting solution merges, filters, is concentrated into 1/3 volume, obtains concentrated solution;
(2) to acetic acid solution (the quality volume fraction that adds 1% chitin in concentrated solution obtained above, that is: in 100ml acetic acid solution, contain 1g chitin), add-on is 1~3%(volume fraction), stir, stratification, visible fluid surface forms the floating matter of well-defined redness, and lower floor's liquid is become faint yellow by redness, lower floor's liquid is emitted, obtain red floating matter;
(3) to the dehydrated alcohol that adds 10~20 times (volume multiples) in red floating matter, occur immediately white precipitate, leave standstill, the red ethanol that filters clear and brightly, steams except without alcohol, obtains red paste, i.e. astaxanthin and ester thereof.
The white precipitate obtaining in described step (3) is chitin (containing a small amount of impurity) that 1.1g adds the proportion relation of 99ml acetic acid to add acetic acid by white precipitate (dry weight), stirring and dissolving, filter, remove impurity, be repeatedly used chitin acetic acid solution.
The method of extracting astaxanthin and ester thereof from krill of the present invention, taking freezing krill as raw material, with extraction using alcohol, process is simple; In the process of preparing wash-out astaxanthin and ester thereof from red floating matter, still use ethanol, whole process is used nontoxic single solvent, make solvent recuperation production technique simple, and chitin can Reusability.Krill after extraction can be used further to produce other products.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1:
Freezing krill 500g, adds 95% ethanol 600ml, stirs and extracts 3h, after leaving standstill, drenches 300ml supernatant liquor, then adds 300ml 95% ethanol continuation stirring to extract 3h.After leaving standstill, pour out 300ml supernatant liquor, then add 300ml 95% ethanol to continue to stir extraction 3h.Whole slag liquid is poured out and squeezed filter, merge 3 liquid 1200ml that filters to get filtrate.Filtrate is concentrated into 400ml.Add wherein 1% chitin acetic acid solution 4ml, stir and leave standstill.Liquid upper strata is red floating matter.Lower floor's liquid becomes faint yellow because redness is adsorbed.Emit lower floor's liquid, make red floating matter 8ml.Add wherein the dehydrated alcohol of 80ml, stir wash-out and leave standstill and filter to obtain red ethanol and white precipitate.
Ethanol in red ethanol is steamed and removed, obtain red paste, i.e. astaxanthin and ester thereof.Gained white precipitate adds 99 parts of acetic acid (V) by 1.1 parts (W), and stirring and dissolving is filtered, and absorption capable of circulation is used.
Embodiment 2:
Extracting method is with embodiment 1, and solvent for use is that the freezing krill of every 500g adds 500ml dehydrated alcohol.It is 1200ml that gained always extracts liquid measure, in the time that extracting solution is concentrated into 400ml, adds 12ml 1% chitin acetic acid solution.Press embodiment, 1 method can make the red floating matter of 14ml, adds wherein 280ml ethanol.Can make red clear and bright ethanolic soln by embodiment 1 method, steaming removes ethanol and obtains red paste, i.e. astaxanthin and ester thereof.The precipitation treatment method of gained white is with embodiment 1, and the chitin acetic acid solution obtaining can be recycled.
Embodiment 3:
Extracting method is with embodiment 1, and solvent for use is that the freezing krill of every 500g adds 700ml 98% ethanol.It is 1200ml that gained always extracts liquid measure, in the time that extracting solution is concentrated into 400ml, adds 8ml 1% chitin acetic acid solution.Press embodiment, 1 method can make the red floating matter of 10ml, adds wherein 150ml ethanol.Can make red clear and bright ethanolic soln by embodiment 1 method, steaming removes ethanol and obtains red paste, i.e. astaxanthin and ester thereof.The precipitation treatment method of gained white is with embodiment 1, and the chitin acetic acid solution obtaining can be recycled.

Claims (3)

1. one kind is extracted the method for astaxanthin and ester thereof from krill, it is characterized in that: step is as follows: freezing krill 500g, add 95% ethanol 600ml, stir and extract 3h, after leaving standstill, drench 300ml supernatant liquor, then add 300ml95% ethanol to continue to stir extraction 3h; After leaving standstill, pour out 300ml supernatant liquor, then add 300ml95% ethanol to continue to stir extraction 3h; Whole slag liquid is poured out and squeezed filter, merge 3 liquid 1200ml that filters to get filtrate; Filtrate is concentrated into 400ml; Add wherein 1% chitin acetic acid solution 4ml, stir and leave standstill; Liquid upper strata is red floating matter, and lower floor's liquid becomes faint yellow because redness is adsorbed; Emit lower floor's liquid, make red floating matter 8ml, add wherein the dehydrated alcohol of 80ml, stir wash-out and leave standstill and filter to obtain red ethanol and white precipitate; Ethanol in red ethanol is steamed and removed, obtain red paste, i.e. astaxanthin and ester thereof; Gained white precipitate adds 99 parts of acetic acid by 1.1 parts, and the umber of white precipitate is weight part, and the umber of acetic acid is parts by volume, and stirring and dissolving is filtered, and absorption capable of circulation is used.
2. one kind is extracted the method for astaxanthin and ester thereof from krill, it is characterized in that: step is as follows: freezing krill 500g, add dehydrated alcohol 500ml, stir and extract 3h, after leaving standstill, drench 300ml supernatant liquor, then add 300ml95% ethanol to continue to stir extraction 3h; After leaving standstill, pour out 300ml supernatant liquor, then add 300ml95% ethanol to continue to stir extraction 3h; Whole slag liquid is poured out and squeezed filter, merge 3 liquid 1200ml that filters to get filtrate; Filtrate is concentrated into 400ml; Add wherein 1% chitin acetic acid solution 12ml, stir and leave standstill; Liquid upper strata is red floating matter, and lower floor's liquid becomes faint yellow because redness is adsorbed; Emit lower floor's liquid, make red floating matter 14ml, add wherein the ethanol of 280ml, stir wash-out and leave standstill and filter to obtain red ethanol and white precipitate; Ethanol in red ethanol is steamed and removed, obtain red paste, i.e. astaxanthin and ester thereof; Gained white precipitate adds 99 parts of acetic acid by 1.1 parts, and the umber of white precipitate is weight part, and the umber of acetic acid is parts by volume, and stirring and dissolving is filtered, and absorption capable of circulation is used.
3. one kind is extracted the method for astaxanthin and ester thereof from krill, it is characterized in that: step is as follows: freezing krill 500g, add 98% ethanol 700ml, stir and extract 3h, after leaving standstill, drench 300ml supernatant liquor, then add 300ml95% ethanol to continue to stir extraction 3h; After leaving standstill, pour out 300ml supernatant liquor, then add 300ml95% ethanol to continue to stir extraction 3h; Whole slag liquid is poured out and squeezed filter, merge 3 liquid 1200ml that filters to get filtrate; Filtrate is concentrated into 400ml; Add wherein 1% chitin acetic acid solution 8ml, stir and leave standstill; Liquid upper strata is red floating matter, and lower floor's liquid becomes faint yellow because redness is adsorbed; Emit lower floor's liquid, make red floating matter 10ml, add wherein the ethanol of 150ml, stir wash-out and leave standstill and filter to obtain red ethanol and white precipitate; Ethanol in red ethanol is steamed and removed, obtain red paste, i.e. astaxanthin and ester thereof; Gained white precipitate adds 99 parts of acetic acid by 1.1 parts, and the umber of white precipitate is weight part, and the umber of acetic acid is parts by volume, and stirring and dissolving is filtered, and absorption capable of circulation is used.
CN201210249101.3A 2012-07-18 2012-07-18 Extraction method of astaxanthin and ester thereof from antarctic krill Expired - Fee Related CN102731359B (en)

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CN102899165B (en) * 2012-10-25 2014-03-12 山东师范大学 Technology for extracting bright red shrimp oil crude product from euphausia superba
CN103864656B (en) * 2014-03-03 2016-05-11 山东师范大学 The method of astaxanthin one ester of astaxanthin odd-numbered fatty acid one ester is rich in preparation

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