CN110003070A - A method of astaxanthin is extracted using ion liquid microemulsion - Google Patents
A method of astaxanthin is extracted using ion liquid microemulsion Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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Abstract
The invention discloses a kind of methods for extracting astaxanthin using ion liquid microemulsion, it include: by ionic liquid, emulsifier and water mixed preparing ion liquid microemulsion, the mass fraction 12~20% of the ion liquid microemulsion intermediate ion liquid made, the mass fraction of emulsifier are 30~60%；It is extracted after shrimp shell meal is mixed with the ion liquid microemulsion；It will be separated by solid-liquid separation through the mixture extracted, and collect liquid to get Astaxanthin extraction liquid is arrived；Add water into the Astaxanthin extraction liquid, stands anti-precipitating astaxanthin, then be separated by solid-liquid separation, collect astaxanthin sediment and drying.The easy to operate of astaxanthin is extracted using extracting method of the present invention, mild condition, extraction time is short, and the extracted amount that astaxanthin is extracted from shrimp shell is high.
Description
Technical field
The present invention relates to chemical extraction technical fields, extract shrimp using ion liquid microemulsion in particular to a kind of
The method of green element.
Background technique
Astaxanthin is a kind of highest carotenoid of value, currently, 90% or more astaxanthin passes through chemistry in market
Synthesis obtains, and has been noted in food safety, product genotoxic potential and sustainability that there are serious risks.Astaxanthin is wide
It is general to be present in different kind organism resource, such as algae, yeast, shellfish shell and flamingo feather.Therefore, from natural raw
The research that astaxanthin is extracted in goods and materials source is of increasing concern.In shrimp process, shrimp head, shrimp shell, shrimp tail account for the total matter of full shrimp
The 40~60% of amount.Natural astaxanthin is recycled from shrimp processing waste, can not only alleviate direct emission waste to environment
Pollution, and the economic value of shrimp processing byproduct can be improved.
Summary of the invention
The present invention provides a kind of method for extracting astaxanthin using ion liquid microemulsion, the inventors discovered that by ionic liquid
Body, emulsifier and water are co-continuous than the microstructure for the ion liquid microemulsion system that mixed preparing obtains by certain mass
Type not only has very strong astaxanthin dissolution characteristics, but also can effectively destroy the microstructure of shrimp shell densification, and shrimp shell is presented
Broken, uneven, porous feature migrates to be conducive to astaxanthin inside shrimp shell into ion liquid microemulsion.The present invention
Astaxanthin is extracted using ion liquid microemulsion, only the comprehensive utilization of shrimp processing byproduct does not provide a kind of new approach, and
Effectively improve the recovery rate of the astaxanthin in prawn processing byproduct shrimp shell.
It is as follows that the present invention provides technical solution:
A method of astaxanthin is extracted using ion liquid microemulsion, comprising:
By ionic liquid, emulsifier and water mixed preparing ion liquid microemulsion, in the ion liquid microemulsion made
The mass fraction of ionic liquid is 12~20%, and the mass fraction of emulsifier is 30~60%；
Ultrasound on extracting is carried out after shrimp shell meal is mixed with the ion liquid microemulsion；
It will be separated by solid-liquid separation through the mixture extracted, and collect liquid to get Astaxanthin extraction liquid is arrived；
Into the Astaxanthin extraction liquid plus then water, the anti-precipitating astaxanthin of standing are separated by solid-liquid separation, collect astaxanthin
Sediment is simultaneously freeze-dried.
Further, the mass ratio of the shrimp shell meal and the ion liquid microemulsion is 1:(40~80).
Further, the shrimp shell meal is obtained by shrimp shell is successively freeze-dried, grinding and 40~120 mesh screens excessively
It arrives.
Further, the ionic liquid include one of tetrabutyl trifluoroacetic acid phosphine and tetrabutyl tetrafluoro boric acid phosphine or
Two kinds.
Further, ultrasound on extracting is used in the extraction process.
Further, when the ultrasound on extracting, ultrasonic power is 50~100W, and ultrasonic time is 30~60min.
Further, the emulsifier includes surfactant and auxiliary agent, the matter of the surfactant and the auxiliary agent
Amount is than being (3~7): 1.
Further, the surfactant is Triton X-100, sorbitan fatty acid ester and polyoxy
One or more of ethylene sorbitan fatty acid ester；The auxiliary agent is one in ethyl alcohol, propyl alcohol, n-butanol and n-amyl alcohol
Kind is several.
Further, in Xiang Suoshu Astaxanthin extraction liquid plus water volume be the Astaxanthin extraction liquid volume 20~
40 times；The time of the standing be 12~for 24 hours.
Further, the separation of solid and liquid is using centrifuge separation；The centrifugal rotational speed be 8000~12000rpm, it is described from
The heart time is 10~20min.
Compared with prior art, the beneficial effect of a kind of method for extracting astaxanthin using ion liquid microemulsion of the invention
Fruit is:
The present invention prepares bicontinuous ionic liquid micro emulsion by the way that ionic liquid, emulsifier and water to be mixed in a certain ratio
Liquid has very strong astaxanthin dissolubility；The ion liquid microemulsion is mixed with shrimp shell meal, can effectively destroy shrimp shell densification
Microstructure migrates into ion liquid microemulsion conducive to shrimp shell inside astaxanthin, improves the recovery rate of astaxanthin；Then through solid
Liquid is collected after liquid separation and arrives Astaxanthin extraction liquid to obtain the final product, recycles astaxanthin to be insoluble in the characteristic of water, to Astaxanthin extraction liquid
In plus water, it is counter to precipitate astaxanthin, it is final to be separated by solid-liquid separation, collect astaxanthin sediment and be simultaneously drying to obtain astaxanthin powder.On the one hand,
Using extracting method safety easy to operate of the invention, can be carried out using conventional equipment, can scale extract astaxanthin, it is another
Aspect extracts the mild condition of astaxanthin using the extracting method, and extraction time is short, avoids the degradation of astaxanthin, protects
The bioactivity of astaxanthin, and the recovery rate of the astaxanthin extracted from shrimp shell is high.
To enable the above objects, features and advantages of the present invention to be clearer and more comprehensible, preferred embodiment is cited below particularly, makees detailed
It is described as follows.
Detailed description of the invention
Fig. 1 is a kind of phasor of ion liquid microemulsion system at 25 DEG C, the ion liquid microemulsion system intermediate ion liquid
Body is tetrabutyl trifluoroacetic acid phosphine, and emulsifier is the mixture that Triton X-100 and n-butanol are 3:1 in mass ratio,
Wherein I is two-phase section, and II is monophase field (micro emulsion liquid zone)；
Fig. 2 is the microscopic appearance scanning electron microscope (SEM) photograph (20000 times of amplification) of the shrimp shell raw material of the embodiment of the present invention 2；
The microscopic appearance scanning electron microscope (SEM) photograph of shrimp shell residue of the Fig. 3 to obtain after the extracted astaxanthin of the embodiment of the present invention 2 (is put
It is 20000 times big)；
Fig. 4 is the high-efficient liquid phase chromatogram of astaxanthin standard items；
Fig. 5 is the high-efficient liquid phase chromatogram for the Astaxanthin extraction liquid that the embodiment of the present invention 2 obtains.
Specific embodiment
To facilitate the understanding of the present invention, it elaborates below with reference to the mode of embodiment to technical solution of the present invention,
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention.
But the invention can be embodied in many other ways as described herein, those skilled in the art can be with
Similar improvement is done without violating the connotation of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Unless otherwise defined, all technologies used herein and scientific term have and the common skill of fields of the present invention
The normally understood identical meaning of art personnel.When there is a conflict, the definition in this specification shall prevail.
The present invention provides a kind of methods for extracting astaxanthin using ion liquid microemulsion, comprising the following steps:
(1) by ionic liquid, emulsifier and water mixed preparing ion liquid microemulsion, the ion liquid microemulsion made
The mass fraction of intermediate ion liquid is 12~20%, and the mass fraction of emulsifier is 30~60%.
The mass fraction of above-mentioned ion liquid microemulsion intermediate ion liquid is specific enumerable be 12%, 15%, 18% or
20% etc.；The specific enumerable mass fraction of emulsifier is 30%, 40%, 50% or 60% etc.；Remaining is water.
Preferably, the ionic liquid be tetrabutyl trifluoroacetic acid phosphine and tetrabutyl tetrafluoro boric acid phosphine in any one or
The mixture of the two in any proportion.
It should be noted that tetrabutyl trifluoroacetic acid phosphine and tetrabutyl tetrafluoro boric acid phosphine are quaternary phosphonium salt ionic liquid, by
Not only thermo-chemical stability is high for the mixture of its kind of one or both and emulsifier and the ion liquid microemulsion of water mixed preparing,
Environmental pollution is small, and has good nonpolarity, has powerful solvability to lipophilicity astaxanthin.
Preferably, the emulsifier includes surfactant and auxiliary agent, the quality of the surfactant and the auxiliary agent
Than for 3~7:1 such as 3:1,4:1,5:1,6:1 or 7:1 etc..
Preferably, the surfactant is Triton X-100, sorbitan fatty acid ester and polyoxy second
Any one in alkene sorbitan fatty acid ester (Tween 80), or Triton X-100, Sorbitan
Any two or three in any proportion mixed in alcohol fatty acid ester and polyoxyethylene sorbitan monooleate (Tween 80)
Close object.
Preferably, the auxiliary agent is one or more of ethyl alcohol, propyl alcohol, n-butanol and n-amyl alcohol, i.e. the auxiliary agent can be with
For any one in ethyl alcohol, propyl alcohol, n-butanol and n-amyl alcohol, or in ethyl alcohol, propyl alcohol, n-butanol and n-amyl alcohol extremely
Few two kinds of mixtures in any proportion.
(2) it is extracted after mixing shrimp shell meal with the ion liquid microemulsion.
Preferably, above-mentioned shrimp shell meal is by being freeze-dried 24 under the conditions of cryogenic temperature is -60~-50 DEG C for new fresh shrimp shell
After~48h, then 40~120 mesh screens of pulverizing obtain.Shrimp shell can be South America prawn, the red shrimp of krill or Argentina
Deng shrimp shell.
Preferably, above-mentioned shrimp shell meal and ion liquid microemulsion are 1:(40~80 in mass ratio) such as 1:40,1:60 or 1:
80 are mixed, and are subsequently placed in ultrasonic cleaning machine and are carried out ultrasound on extracting.
Preferably, ultrasound on extracting is used in the extraction process.
It should be noted that extraction process is assisted using ultrasonic wave, shrimp shell meal and ion liquid microemulsion can be strengthened
Contact, to be conducive to the dissolution of astaxanthin.The ultrasound on extracting process carries out at normal temperature, it is preferable that ultrasound on extracting
In the process, the ultrasonic power that ultrasonic cleaning machine is arranged is 50~100W；Ultrasonic time is 30~60min.
(3) it will be separated by solid-liquid separation through the extraction mixture extracted, and collect liquid, which is that astaxanthin mentions
Take liquid.
It should be noted that above-mentioned separation of solid and liquid be will be extracted astaxanthin shrimp shell meal residue and extracted shrimp blueness
The ion liquid microemulsion of element is separated.Preferably, above-mentioned separation of solid and liquid is preferably centrifuged using centrifuge, centrifugation
Revolving speed is 8000~12000rpm, and centrifugation time is 5~10min.Certainly, above-mentioned separation of solid and liquid can also take suction filtration mode to carry out
It is separated by solid-liquid separation.
(4) add water in Xiang Suoshu Astaxanthin extraction liquid, stand anti-precipitating astaxanthin, then obtained solidliquid mixture is carried out
It is separated by solid-liquid separation, collects astaxanthin sediment and drying.
It should be noted that Astaxanthin extraction liquid is the mixture of ion liquid microemulsion and astaxanthin, when to astaxanthin
In extracting solution plus when water, dissolubility of the astaxanthin in ion liquid microemulsion can be reduced, astaxanthin is precipitated；Preferably, add
Water volume is 25~40 times such as 25 times, 28 times, 30 times, 35 times or 40 times of Astaxanthin extraction liquid product.Add after water in room temperature
It is lower stand 12~for 24 hours such as 12h, 15h, 18h, 20h or for 24 hours, then be separated by solid-liquid separation.The separation of solid and liquid is it is also preferred that using centrifuge
It is centrifuged, centrifugal rotational speed is 8000~12000rpm, and centrifugation time is 10~20min；The bottom obtained by centrifugation
Sediment is astaxanthin sediment；Finally cryogenic temperature be -60~-50 DEG C, cooling time be 24~48h under conditions of into
Row is freeze-dried up to astaxanthin powder.
It should be noted that above-mentioned water preferably uses distilled water, naturally it is also possible to use deionized water, pure water or ultrapure
Water.
The present invention prepares bicontinuous ionic liquid micro emulsion by the way that ionic liquid, emulsifier and water to be mixed in a certain ratio
Liquid has very strong astaxanthin dissolubility；The ion liquid microemulsion is mixed with shrimp shell meal, can effectively destroy shrimp shell densification
Microstructure migrates into ion liquid microemulsion conducive to shrimp shell inside astaxanthin, improves the recovery rate of astaxanthin；Then through solid
Liquid is collected after liquid separation and arrives Astaxanthin extraction liquid to obtain the final product, recycles astaxanthin to be insoluble in the characteristic of water, to Astaxanthin extraction liquid
In plus water, it is counter to precipitate astaxanthin, it is final to be separated by solid-liquid separation, collect astaxanthin sediment and be simultaneously drying to obtain astaxanthin powder.On the one hand,
Using extracting method safety easy to operate of the invention, can be carried out using conventional equipment, can scale extract astaxanthin, it is another
Aspect extracts the mild condition of astaxanthin using the extracting method, and extraction time is short, avoids the degradation of astaxanthin, protects
The bioactivity of astaxanthin, and the recovery rate of the astaxanthin extracted from shrimp shell is high.
To facilitate the understanding of the present invention, below with reference to embodiment to further illustrate the technical scheme of the present invention.
Embodiment 1
(1) it is first freeze-dried for 24 hours under the conditions of -60 DEG C of cryogenic temperatures after cleaning new fresh shrimp shell, is subsequently placed in grinder
It is spare to obtain shrimp shell meal after 40 mesh mesh screens for middle grind into powder.
(2) ionic liquid, emulsifier and distilled water are uniformly mixed and prepare ion liquid microemulsion, the ionic liquid made
The mass fraction of body microemulsion intermediate ion liquid is 12%, and the mass fraction of emulsifier is 30%, remaining is distilled water；Wherein,
Ionic liquid is tetrabutyl trifluoroacetic acid phosphine, and emulsifier by being 3 by Triton X-100 and n-butanol in mass ratio:
1, which carries out uniformly mixed prepare, obtains.
(3) ion liquid microemulsion that the shrimp shell meal and 40g step (2) for taking 1g step (1) to obtain obtain is placed in centrifuge tube
In, it is stirred, then the centrifuge tube is placed in ultrasonic cleaning machine, set ultrasonic power as 50W, room temperature ultrasound 60min,
Under ultrasonic wave added effect, ion liquid microemulsion is promoted to extract the astaxanthin in shrimp shell meal.
(4) the extraction mixture obtained through step (3) is placed in a centrifuge, is centrifuged under the centrifugal rotational speed of 8000rpm
20min obtains the ion liquid microemulsion and shrimp shell meal residue precipitating of astaxanthin-containing, collects liquid, that is, Astaxanthin extraction liquid.
(5) distilled water that 40 times of Astaxanthin extraction liquid product is added in obtained Astaxanthin extraction liquid is collected to step (4),
After being stirred, 12h is stood at room temperature, precipitates astaxanthin, is then consolidated obtained solidliquid mixture using centrifuge
Liquid separation, the revolving speed of centrifuge are set as 8000rpm, centrifugation time 20min, and it is green to regather the bottom shrimp obtained by centrifugation
Plain sediment is freeze-dried 48h under the conditions of -50 DEG C of cryogenic temperatures finally to get powdered astaxanthin is arrived.
Embodiment 2
(1) it first is freeze-dried 36h under the conditions of -55 DEG C of cryogenic temperatures after cleaning new fresh shrimp shell, is subsequently placed in grinder
It is spare to obtain shrimp shell meal after 80 mesh mesh screens for middle grind into powder.
(2) ionic liquid, emulsifier and distilled water are uniformly mixed and prepare ion liquid microemulsion, the ionic liquid made
The mass fraction of body microemulsion intermediate ion liquid is 15%, and the mass fraction of emulsifier is 50%, remaining is distilled water；Wherein,
Ionic liquid is tetrabutyl tetrafluoro boric acid phosphine, and emulsifier by being that 5:1 mix by Tween 80 and n-amyl alcohol in mass ratio
Even preparation obtains.
(3) ion liquid microemulsion that the shrimp shell meal and 60g step (2) for taking 1g step (1) to obtain obtain is placed in centrifuge tube
In, it is stirred, then the centrifuge tube is placed in ultrasonic cleaning machine, set ultrasonic power as 70W, room temperature ultrasound 40min,
Under ultrasonic wave added effect, ion liquid microemulsion is promoted to extract the astaxanthin in shrimp shell meal.
(4) the extraction mixture obtained through step (3) is placed in a centrifuge, is centrifuged under the centrifugal rotational speed of 12000rpm
10min obtains the supernatant and shrimp shell meal residue precipitating of the ion liquid microemulsion of astaxanthin-containing, collects liquid, that is, astaxanthin
Extracting solution.
(5) distilled water that 25 times of Astaxanthin extraction liquid product is added in obtained Astaxanthin extraction liquid is collected to step (4),
After being stirred, 16h is stood at room temperature, precipitates astaxanthin, is then consolidated obtained solidliquid mixture using centrifuge
Liquid separation, the revolving speed of centrifuge are set as 12000rpm, centrifugation time 10min, regather the bottom shrimp obtained by centrifugation
Green element sediment is freeze-dried 36h under the conditions of -50 DEG C of cryogenic temperatures finally to get powdered astaxanthin is arrived.
Embodiment 3
(1) it first is freeze-dried 48h under the conditions of -50 DEG C of cryogenic temperatures after cleaning new fresh shrimp shell, is subsequently placed in grinder
It is spare to obtain shrimp shell meal after 120 mesh mesh screens for middle grind into powder.
(2) ionic liquid, emulsifier and distilled water are uniformly mixed and prepare ion liquid microemulsion, the ionic liquid made
The mass fraction of body microemulsion intermediate ion liquid is 20%, and the mass fraction of emulsifier is 40%, remaining is distilled water；Wherein,
Ionic liquid is tetrabutyl tetrafluoro boric acid phosphine, and emulsifier by being 7 by sorbitan mono-laurate and ethyl alcohol in mass ratio:
1, which carries out uniformly mixed prepare, obtains.
(3) ion liquid microemulsion that the shrimp shell meal and 80g step (2) for taking 1g step (1) to obtain obtain is placed in centrifuge tube
In, it is stirred, then the centrifuge tube is placed in ultrasonic cleaning machine, set ultrasonic power as 100W, room temperature ultrasound 30min,
Under ultrasonic wave added effect, ion liquid microemulsion is promoted to extract the astaxanthin in shrimp shell meal.
(4) the extraction mixture obtained through step (3) is placed in a centrifuge, is centrifuged under the centrifugal rotational speed of 10000rpm
15min obtains the supernatant and shrimp shell meal residue precipitating of the ion liquid microemulsion of astaxanthin-containing, collects liquid, that is, astaxanthin
Extracting solution.
(5) water that 30 times of Astaxanthin extraction liquid product is added in obtained Astaxanthin extraction liquid, stirring are collected to step (4)
After mixing, 18h is stood at room temperature, precipitates astaxanthin, and obtained solidliquid mixture is then subjected to solid-liquid point using centrifuge
From the revolving speed of centrifuge is set as 8000rpm, centrifugation time 10min, and it is heavy to regather the bottom astaxanthin obtained by centrifugation
Starch is freeze-dried 48h under the conditions of -50 DEG C of cryogenic temperatures finally to get powdered astaxanthin is arrived.
Embodiment 4
(1) it first is freeze-dried 32h under the conditions of -60 DEG C of cryogenic temperatures after cleaning new fresh shrimp shell, is subsequently placed in grinder
It is spare to obtain shrimp shell meal after 60 mesh mesh screens for middle grind into powder.
(2) ionic liquid, emulsifier and distilled water are uniformly mixed and prepare ion liquid microemulsion, the ionic liquid made
The mass fraction of body microemulsion intermediate ion liquid is 15%, and the mass fraction of emulsifier is 40%, remaining is distilled water；Wherein,
Ionic liquid is tetrabutyl trifluoroacetic acid phosphine and tetrabutyl tetrafluoro boric acid phosphine is the mixture of 1:1 in mass ratio, and emulsifier passes through
By Triton X-100 and n-butanol be in mass ratio 3:1 carry out be uniformly mixed prepare obtain.
(3) ion liquid microemulsion that the shrimp shell meal and 50g step (2) for taking 1g step (1) to obtain obtain is placed in centrifuge tube
In, it is stirred, then the centrifuge tube is placed in ultrasonic cleaning machine, set ultrasonic power as 80W, room temperature ultrasound 40min,
Under ultrasonic wave added effect, ion liquid microemulsion is promoted to extract the astaxanthin in shrimp shell meal.
(4) the extraction mixture obtained through step (3) is placed in a centrifuge, is centrifuged under the centrifugal rotational speed of 9000rpm
18min obtains the supernatant and shrimp shell meal residue precipitating of the ion liquid microemulsion of astaxanthin-containing, collects supernatant, as
Astaxanthin extraction liquid.
(5) water that 40 times of Astaxanthin extraction liquid product is added in obtained Astaxanthin extraction liquid, stirring are collected to step (4)
After mixing, 12h is stood at room temperature, precipitates astaxanthin, and obtained solidliquid mixture is then subjected to solid-liquid point using centrifuge
From the revolving speed of centrifuge is set as 8000rpm, centrifugation time 20min, and it is heavy to regather the bottom astaxanthin obtained by centrifugation
Starch is freeze-dried 48h under the conditions of -50 DEG C of cryogenic temperatures finally to get powdered astaxanthin is arrived.
Embodiment 5
(1) it first is freeze-dried 48h under the conditions of -50 DEG C of cryogenic temperatures after cleaning new fresh shrimp shell, is subsequently placed in grinder
It is spare to obtain shrimp shell meal after 100 mesh mesh screens for middle grind into powder.
(2) ionic liquid, emulsifier and distilled water are uniformly mixed and prepare ion liquid microemulsion, the ionic liquid made
The mass fraction of body microemulsion intermediate ion liquid is 18%, and the mass fraction of emulsifier is 60%, remaining is distilled water；Wherein,
Ionic liquid is tetrabutyl trifluoroacetic acid phosphine and tetrabutyl tetrafluoro boric acid phosphine is the mixture of 2:1 in mass ratio, and emulsifier passes through
By Triton X-100 and n-butanol be in mass ratio 6:1 carry out be uniformly mixed prepare obtain.
(3) ion liquid microemulsion that the shrimp shell meal and 40g step (2) for taking 1g step (1) to obtain obtain is placed in centrifuge tube
In, it is stirred, then the centrifuge tube is placed in ultrasonic cleaning machine, set ultrasonic power as 90W, room temperature ultrasound 40min,
Under ultrasonic wave added effect, ion liquid microemulsion is promoted to extract the astaxanthin in shrimp shell meal.
(4) the extraction mixture obtained through step (3) is placed in a centrifuge, is centrifuged under the centrifugal rotational speed of 11000rpm
18min obtains the supernatant of the ion liquid microemulsion of shrimp shell meal residue and astaxanthin-containing, collects the liquid i.e. astaxanthin and mentions
Take liquid.
(5) water that 20 times of Astaxanthin extraction liquid product is added in obtained Astaxanthin extraction liquid, stirring are collected to step (4)
It after mixing, stands at room temperature for 24 hours, precipitates astaxanthin, obtained solidliquid mixture is then subjected to solid-liquid point using centrifuge
From the revolving speed of centrifuge is set as 10000rpm, centrifugation time 15min, regathers the bottom astaxanthin obtained by centrifugation
Sediment is freeze-dried 36h under the conditions of -50 DEG C of cryogenic temperatures finally to get powdered astaxanthin is arrived.
Comparative example 1
The difference from example 2 is that: use the ionic liquid of ionic liquid and distilled water in mass ratio for 1:9 mixed preparing
Body aqueous solution replaces ion liquid microemulsion, the other the same as in Example 2.
Comparative example 2
The difference from example 2 is that: ion liquid microemulsion, the other the same as in Example 2 are replaced using organic solvent ethyl alcohol.
Comparative example 3
The difference from example 2 is that: ion liquid microemulsion, the other the same as in Example 2 are replaced using organic solvent-acetone.
Comparative example 4
The difference from example 2 is that: ion liquid microemulsion is replaced using organic solvent dichloromethane, it is other with implementation
Example 2.
Comparative example 5
The difference from example 2 is that: it is micro- using individual ionic liquid tetrabutyl tetrafluoro boric acid phosphine replacement ionic liquid
Lotion, the other the same as in Example 2.
Comparative example 6
The difference from example 2 is that: ionic liquid four is replaced using -3 methylimidazole acetate of ionic liquid 1- ethyl
Butyl tetrafluoro boric acid phosphine, the other the same as in Example 2.
Comparative example 7
The difference from example 2 is that: in step (2), make to prepare obtained ion liquid microemulsion intermediate ion liquid
Mass fraction is 30%, the other the same as in Example 2.
Comparative example 8
The difference from example 2 is that: in step (2), make to prepare obtained ion liquid microemulsion intermediate ion liquid
Mass fraction is 2%, the other the same as in Example 2.
If Fig. 1 is a kind of phasor of ion liquid microemulsion system at 25 DEG C, the ion liquid microemulsion system intermediate ion
Liquid is tetrabutyl trifluoroacetic acid phosphine ([P4444]CF3COO), emulsifier is Triton X-100 (TX-100) He Zhengding
Alcohol (n-butanol) is the mixture of 3:1 in mass ratio, wherein I is two-phase section, II is monophase field (micro emulsion liquid zone)；By the Fig. 1
It is found that the ion liquid microemulsion prepared using the ratio range of ionic liquid of the invention, emulsifier and water can just obtain
To the ion liquid microemulsion of stable and uniform, can the astaxanthin preferably in prawn shell extracted.
Such as the microscopic appearance scanning electron microscope (SEM) photograph (20000 times of amplification) for the shrimp shell raw material that Fig. 2 is the embodiment of the present invention 2, Fig. 3 is
The microscopic appearance scanning electron microscope (SEM) photograph (20000 times of amplification) of the shrimp shell residue obtained after the extracted astaxanthin of the embodiment of the present invention 2, needs
It is noted that the embodiment of the present invention 1 and 3-5 use identical shrimp shell raw material, and obtained after obtained extracted astaxanthin
The shrimp shell residue obtained after the microscopic appearance scanning electron microscope (SEM) photograph of shrimp shell residue and the extracted astaxanthin of the embodiment of the present invention 2 it is microcosmic
Topography scan electron microscope is essentially identical；Shrimp shell known to Fig. 2 and Fig. 3 by ion liquid microemulsion processing is destructurized,
Concave-convex and porous structure is presented.
Fig. 4 is the high-efficient liquid phase chromatogram of astaxanthin standard items, and Fig. 5 is the Astaxanthin extraction that the embodiment of the present invention 2 obtains
The high-efficient liquid phase chromatogram of liquid.Peak retention time both it can be seen from Fig. 4 and Fig. 5 is completely the same, and without it in Fig. 5
His miscellaneous peak, it is possible thereby to prove, the extract that the embodiment of the present invention 2 obtains is astaxanthin.It should be noted that the present invention is implemented
The high-efficient liquid phase chromatogram base for the astaxanthin that the high-efficient liquid phase chromatogram and embodiment 1 for the astaxanthin that example 1 and 3~5 obtains obtain
This is identical, and equally, the extract that the embodiment of the present invention 1 and 3~5 obtains is astaxanthin.
The extracted amount of astaxanthin in above-described embodiment 1~5 and comparative example 1~8 is calculated, as a result as shown in table 1 below.
The calculation formula of the extracted amount of astaxanthin is as follows:
Extracted amount (μ g/g)=extraction astaxanthin total amount (μ g)/shrimp shell butt quality (g).
Table 1
| Project | Extracted amount (μ g/g) |
| Embodiment 1 | 34.2±0.3 |
| Embodiment 2 | 38.6±0.5 |
| Embodiment 3 | 39.8±0.4 |
| Embodiment 4 | 32.7±0.1 |
| Embodiment 5 | 36.8±0.3 |
| Comparative example 1 | 20.2±0.1 |
| Comparative example 2 | 27.4±0.4 |
| Comparative example 3 | 28.2±0.1 |
| Comparative example 4 | 26.1±0.2 |
| Comparative example 5 | 0 |
| Comparative example 6 | 6.3±0.1 |
| Comparative example 7 | 15.2±0.1 |
| Comparative example 8 | 20.9±0.2 |
From upper 1 result of table:
1, the present invention extracts the extracted amount for obtaining astaxanthin using ion liquid microemulsion compared to using ion from shrimp shell
The extracted amount for the astaxanthin that liquid aqueous solution is extracted from shrimp shell is higher.
2, the present invention extracts the extracted amount for obtaining astaxanthin using ion liquid microemulsion compared to using organic from shrimp shell
The extracted amount for the astaxanthin that solvent is extracted from shrimp shell is higher.
3, astaxanthin can not be extracted using individual ionic liquid tetrabutyl tetrafluoro boric acid phosphine, because of nearly its viscosity at room temperature
It is very big, it is unfavorable for mass transfer.
4, microemulsion system, mixture pair can not be constituted with emulsifier of the invention and water using imidazolium ionic liquid
Astaxanthin dissolubility is poor, is unfavorable for the extraction of astaxanthin.
5, using the ionic liquid prepared other than the ratio range of ionic liquid of the invention, emulsifier and water
Body microemulsion, is unfavorable for the dissolution of astaxanthin, therefore the Astaxanthin extraction amount extracted from shrimp shell is lower.
The above is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, inventive formulation and preparation process can have various modifications and variations.Person of ordinary skill in the field should be bright
, any improvement in the present invention, the addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, concrete mode
Selection etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of method for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: include:
By ionic liquid, emulsifier and water mixed preparing ion liquid microemulsion, the ion liquid microemulsion intermediate ion made
The mass fraction of liquid is 12~20%, and the mass fraction of emulsifier is 30~60%；
It is extracted after shrimp shell meal is mixed with the ion liquid microemulsion；
It will be separated by solid-liquid separation through the mixture extracted, and collect liquid to get Astaxanthin extraction liquid is arrived；
Into the Astaxanthin extraction liquid plus then water, the anti-precipitating astaxanthin of standing are separated by solid-liquid separation, collect astaxanthin precipitating
Object is simultaneously freeze-dried.
2. the method according to claim 1 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: the shrimp
The mass ratio of shell powder and the ion liquid microemulsion is 1:(40~80).
3. the method according to claim 1 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: the shrimp
Shell powder is obtained by shrimp shell is successively freeze-dried, grinding and 40~120 mesh screens excessively.
4. it is according to claim 1 using ion liquid microemulsion extract astaxanthin method, it is characterised in that: it is described from
Sub- liquid includes one or both of tetrabutyl trifluoroacetic acid phosphine and tetrabutyl tetrafluoro boric acid phosphine.
5. the method according to claim 1 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: the extraction
Using ultrasound on extracting during taking.
6. the method according to claim 5 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: described super
When sound auxiliary extraction, ultrasonic power is 50~100W, and ultrasonic time is 30~60min.
7. the method according to claim 1 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: the cream
Agent includes surfactant and auxiliary agent, and the mass ratio of the surfactant and the auxiliary agent is (3~7): 1.
8. the method according to claim 6 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: the table
Face activating agent is in Triton X-100, sorbitan fatty acid ester and polyoxyethylene sorbitan fatty acid ester
One or more；The auxiliary agent is one or more of ethyl alcohol, propyl alcohol, n-butanol and n-amyl alcohol.
9. the method according to claim 1 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: Xiang Suoshu
In Astaxanthin extraction liquid plus the volume of water is 20~40 times of the volume of the Astaxanthin extraction liquid；The time of the standing is 12
~for 24 hours.
10. the method according to claim 1 for extracting astaxanthin using ion liquid microemulsion, it is characterised in that: described
It is separated by solid-liquid separation using centrifuge separation；The centrifugal rotational speed is 8000~12000rpm, and the centrifugation time is 10~20min.
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| CN110317156A (en) * | 2019-08-13 | 2019-10-11 | 广东海洋大学 | A kind of method that depth eutectic solvent microemulsion extracts system and extracts astaxanthin |
| CN111150064A (en) * | 2020-01-11 | 2020-05-15 | 临沂大学 | Preparation method of microcapsule rich in chlorophyll and reduced sulforaphane |
| CN111203195A (en) * | 2020-02-21 | 2020-05-29 | 广东海洋大学 | Biological porous adsorbent, preparation method thereof, water defluorination method and device |
| CN111389046A (en) * | 2020-03-26 | 2020-07-10 | 广东海洋大学 | Extraction agent and method for extracting astaxanthin by using same |
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| CN110317156A (en) * | 2019-08-13 | 2019-10-11 | 广东海洋大学 | A kind of method that depth eutectic solvent microemulsion extracts system and extracts astaxanthin |
| CN111150064A (en) * | 2020-01-11 | 2020-05-15 | 临沂大学 | Preparation method of microcapsule rich in chlorophyll and reduced sulforaphane |
| CN111203195A (en) * | 2020-02-21 | 2020-05-29 | 广东海洋大学 | Biological porous adsorbent, preparation method thereof, water defluorination method and device |
| CN111203195B (en) * | 2020-02-21 | 2022-12-23 | 广东海洋大学 | Biological porous adsorbent, preparation method thereof, water defluorination method and device |
| CN111389046A (en) * | 2020-03-26 | 2020-07-10 | 广东海洋大学 | Extraction agent and method for extracting astaxanthin by using same |
| CN111389046B (en) * | 2020-03-26 | 2021-08-24 | 广东海洋大学 | Extraction agent and method for extracting astaxanthin by using same |
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