CN109181864A - A kind of low unsaponifiable matter antarctic krill oil and preparation method thereof - Google Patents

A kind of low unsaponifiable matter antarctic krill oil and preparation method thereof Download PDF

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Publication number
CN109181864A
CN109181864A CN201811290847.2A CN201811290847A CN109181864A CN 109181864 A CN109181864 A CN 109181864A CN 201811290847 A CN201811290847 A CN 201811290847A CN 109181864 A CN109181864 A CN 109181864A
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Prior art keywords
krill oil
antarctic krill
cyclodextrin
unsaponifiable matter
preparation
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CN201811290847.2A
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Chinese (zh)
Inventor
胥亚夫
刘冬梅
赵伟
张庆香
郭忠
吕晶
余奕珂
李宣延
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Liaoyu Antarctic Krill Technology Development Co Ltd
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Liaoyu Antarctic Krill Technology Development Co Ltd
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Priority to CN201811290847.2A priority Critical patent/CN109181864A/en
Publication of CN109181864A publication Critical patent/CN109181864A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/008Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/12Refining fats or fatty oils by distillation

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Meat, Egg Or Seafood Products (AREA)

Abstract

The present invention provides a kind of preparation methods of low unsaponifiable matter antarctic krill oil, comprising: S1. to slightly mention in antarctic krill oil be added concentration 75~99% ethanol solution and be uniformly mixing to obtain mixed liquor;S2. the derivative of cyclodextrin and/or cyclodextrin is added into mixed liquor, stirs and filtrate is obtained by filtration;S3. vacuum distillation removing ethyl alcohol is carried out to filtrate and obtains low unsaponifiable matter antarctic krill oil.The present invention also provides the low unsaponifiable matter antarctic krill oils that preparation method as described above is prepared.The unsaponifiable matter content in antarctic krill oil that the present invention obtains is reduced to 1% hereinafter, content of phospholipid significantly improves the mobility, stability and quality of antarctic krill oil not less than 40%;Used reagent is the very high reagent of safety, meets the production specification of food safety;Preparation method step of the invention is few, easy to operate, can carry out large-scale industrial production, improve production efficiency, saved production cost.

Description

A kind of low unsaponifiable matter antarctic krill oil and preparation method thereof
Technical field
The present invention relates to krill oil extract field, more particularly, to a kind of low unsaponifiable matter antarctic krill oil and Preparation method.
Background technique
About 6.5~1,000,000,000 tons of the total biomass of krill, biological academic year can amount of fishing up to 100,000,000 tons, this year catches The amount of obtaining is equivalent to whole world marine aquatic product year fishing total output.It is most important latent that krill has become world's ocean-going fishing industry In fishery resources.Result of study shows moisture content 77.9%-83.1%, crude protein 11.9%-16.3% in the fresh sample of krill, Crude fat 0.50%-3.6%.Polyunsaturated fat rich in ω -3 series frequently as functional food in krill lipid Acid, Phospholipids, vitamin, astaxanthin etc..In krill lipid polyunsaturated fatty acid (PUFAs) content of ω -3 series compared with Horn of plenty, especially eicosapentaenoic acid (EPA, 20:5), docosahexaenoic acid (DHA, 22:6) account for total fatty acids respectively and contain 15.0%-25.3%, 9.3%-21.2% of amount.Studies have shown that the polyunsaturated fatty acid master of ω -3 series of krill It is present in phosphatide, compared with traditional fish triglycerides lipid, is more conducive to human body for polyunsaturated fatty acid Absorption.Carotenoid substance also rich in krill lipid component, most important of which is that astaxanthin, ice The every 100g of fresh krill about astaxanthin-containing 3-4mg.Astaxanthin can protect lipid material from oxidation, be resisted in nature Oxidation and the elimination strongest natural pigment of free radical ability.The lipid extracted from krill has anti-oxidant, anti-aging, clear Except different physiological roles such as free radical, reducing blood lipid, brain tonic and intelligence developments, and after measured, the lipid of krill will not generate any poison Side effect, health-care efficacy is more comprehensive, is a kind of very wide functional health care food of development prospect.
But there is a problem of that unsaponifiable matter content is high after krill oil extract, unsaponifiable matter content is excessively high to will lead to south Pole krill oil poor fluidity, the problems such as transparency is low, therefore the preparation method for needing a kind of low unsaponifiable matter antarctic krill oil is used In the quality for improving antarctic krill oil.
Summary of the invention
It is an object of the invention to the high defects of the antarctic krill oil unsaponifiable matter content for overcoming the prior art to extract, and mention For a kind of low unsaponifiable matter antarctic krill oil and preparation method thereof.
To achieve the above object, the present invention provides a kind of preparation methods of low unsaponifiable matter antarctic krill oil, including with Lower step:
S1. ethanol solution and mixed liquor is uniformly mixing to obtain to slightly mentioning being added in antarctic krill oil, the ethanol solution Concentration is 75~99%;
S2. the derivative of cyclodextrin and/or cyclodextrin is added into the mixed liquor, stirs and be obtained by filtration filtrate, with The total weight for slightly mentioning antarctic krill oil is counted for 100%, and the additional amount of the derivative of the cyclodextrin and/or cyclodextrin is 5 ~50%;
S3. vacuum distillation removing ethyl alcohol is carried out to the filtrate and obtains low unsaponifiable matter antarctic krill oil.
The present invention also provides the low unsaponifiable matter antarctic krill oils that preparation method as described above is prepared.
According to the present invention, by ethyl alcohol with slightly mention antarctic krill oil and mix, add the derivative of cyclodextrin and/or cyclodextrin It is stirred, can make cyclodextrin and/or cyclodextrin are fully dispersed in mixed liquor to reach more superior adsorption effect, after processing Antarctic krill oil in unsaponifiable matter content be reduced to 1% hereinafter, content of phospholipid be not less than 40%, significantly improve South Pole phosphorus Mobility, stability and the quality of shrimp sauce;Reagent used in the present invention is the very high reagent of safety, meets food peace Full production specification;Preparation method step of the invention is few, easy to operate, can carry out large-scale industrial production, improve Production efficiency has saved production cost.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of preparation methods of low unsaponifiable matter antarctic krill oil, comprising the following steps:
S1. ethanol solution and mixed liquor is uniformly mixing to obtain to slightly mentioning being added in antarctic krill oil, the ethanol solution Concentration is 75~99%;
S2. the derivative of cyclodextrin and/or cyclodextrin is added into the mixed liquor, stirs and be obtained by filtration filtrate, with The total weight for slightly mentioning antarctic krill oil is counted for 100%, and the additional amount of the derivative of the cyclodextrin and/or cyclodextrin is 5 ~50%;
S3. vacuum distillation removing ethyl alcohol is carried out to the filtrate and obtains low unsaponifiable matter antarctic krill oil.
According to the present invention, by ethyl alcohol with slightly mention antarctic krill oil and mix, add the derivative of cyclodextrin and/or cyclodextrin It is stirred, can make cyclodextrin and/or cyclodextrin are fully dispersed in mixed liquor to reach more superior adsorption effect, after processing Antarctic krill oil in unsaponifiable matter content be reduced to 1% hereinafter, content of phospholipid be not less than 40%, significantly improve South Pole phosphorus Mobility, stability and the quality of shrimp sauce;Reagent used in the present invention is the very high reagent of safety, meets food peace Full production specification;Preparation method step of the invention is few, easy to operate, can carry out large-scale industrial production, improve Production efficiency has saved production cost.
Preferably, cyclodextrin described in step S2 can be selected from one of beta-cyclodextrin, alpha-cyclodextrin and gamma-cyclodextrin Or it is a variety of, the derivative of the cyclodextrin can be selected from one in 2-HP-BETA-CD and 2,6- dimethyl-β-cyclodextrin Kind is a variety of;Most preferably, the cyclodextrin can be beta-cyclodextrin with save the cost.
Preferably, in step S1, it is described slightly mention antarctic krill oil and 75~95% ethanol solution w/v (w/ V) it is 1:(1~10), using the w/v on the one hand antarctic krill oil and ethanol solution can make that ground β-is added below Cyclodextrin is fully uniformly dispersed, and on the other hand can reduce distillation ground time and cost.
Preferably, in step S1, the condition of the stirring includes at -4~40 DEG C, with 300~3000rpm stirring 0.1~ 6h。
Preferably, in step S1, the condition of the stirring is included at 20~40 DEG C, with 300~3000rpm stirring 0.5 ~6h.
Preferably, in step S3, the condition of the vacuum distillation is 20~80 DEG C, -0.05~-0.1MPa distillation 0.5~ 6h。
The present invention also provides the low unsaponifiable matter antarctic krill oils being prepared according to above-described preparation method.
Below by embodiment, present invention be described in more detail.Not being saponified for antarctic krill oil is slightly mentioned in following embodiment Object content is 2.3%, content of phospholipid 42.3%.
Embodiment 1
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 100mL 95%, is stirred under the conditions of 20 DEG C, 1000rpm It mixes 0.5h and obtains mixed liquor, 4g beta-cyclodextrin is added into the mixed liquor, 2h is stirred under the conditions of 50 DEG C, 2000rpm, carry out Filtrate is obtained by filtration, distills 0.5h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 19g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.6%, removal efficiency 73.9%, content of phospholipid 43.2%.
Embodiment 2
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 100mL 90%, is stirred under the conditions of -4 DEG C, 1500rpm It mixes 2h and obtains mixed liquor, 4g beta-cyclodextrin is added into the mixed liquor, stirs 2h under the conditions of 50 DEG C, 2000rpm, carried out Filter obtains filtrate, distills 0.5h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 19g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.2%, removal efficiency 91.3%, content of phospholipid 40.5%.
Embodiment 3
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 100mL 80%, is stirred under the conditions of 37 DEG C, 1000rpm It mixes 0.5h and obtains mixed liquor, 4g beta-cyclodextrin is added into the mixed liquor, 2h is stirred under the conditions of 50 DEG C, 3000rpm, carry out Filtrate is obtained by filtration, distills 2h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 19g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.8%, removal efficiency 65.2%, content of phospholipid 43.9%.
Embodiment 4
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 100mL75%, is stirred under the conditions of 25 DEG C, 1000rpm 2h obtains mixed liquor, and 4g beta-cyclodextrin is added into the mixed liquor, stirs 2h under the conditions of 50 DEG C, 2000rpm, is filtered Filtrate is obtained, distills 3h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 19g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.75%, removal efficiency 67.4%, content of phospholipid 42.5%.
Embodiment 5
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 100mL 95%, is stirred under the conditions of 25 DEG C, 3000rpm It mixes 0.5h and obtains mixed liquor, 1g beta-cyclodextrin is added into the mixed liquor, 2h is stirred under the conditions of 50 DEG C, 3000rpm, carry out Filtrate is obtained by filtration, distills 3h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 19.5g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.8%, removal efficiency 65.2%, content of phospholipid 43.2%.
Embodiment 6
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 100mL 95%, is stirred under the conditions of 25 DEG C, 3000rpm It mixes 0.5h and obtains mixed liquor, 6g beta-cyclodextrin is added into the mixed liquor, 2h is stirred under the conditions of 50 DEG C, 3000rpm, carry out Filtrate is obtained by filtration, distills 3h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 19.1g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.6%, removal efficiency 73.9%, content of phospholipid 45%.
Embodiment 7
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 100mL 95%, is stirred under the conditions of 20 DEG C, 200rpm 0.5h obtains mixed liquor, and 10g beta-cyclodextrin is added into the mixed liquor, 2h is stirred under the conditions of 50 DEG C, 1000rpm, carries out Filtrate is obtained by filtration, distills 4h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 18.8g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.6%, removal efficiency 73.9%, content of phospholipid 44.2%.
Embodiment 8
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 20mL 95%, is stirred under the conditions of 20 DEG C, 200rpm 0.5h obtains mixed liquor, and 10g beta-cyclodextrin is added into the mixed liquor, 2h is stirred under the conditions of 50 DEG C, 1000rpm, carries out Filtrate is obtained by filtration, distills 4h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 19g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.8%, removal efficiency 65.2%, content of phospholipid 44.7%.
Embodiment 9
20g is slightly mentioned to antarctic krill oil to mix with the ethanol solution of 200mL 95%, is stirred under the conditions of 20 DEG C, 200rpm 0.5h obtains mixed liquor, and 10g beta-cyclodextrin is added into the mixed liquor, 2h is stirred under the conditions of 50 DEG C, 1000rpm, carries out Filtrate is obtained by filtration, distills 4h under the conditions of 50 DEG C, -0.1MPa, obtains the antarctic krill oil of the low unsaponifiable matter of 18g.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in the present embodiment 0.9%, removal efficiency 60%, content of phospholipid 42%.
Comparative example 1
It weighs 20g and slightly mentions antarctic krill oil, obtain mixed liquor with 80mL food-grade n-hexane dissolution;Beta-cyclodextrin is dissolved in Beta-cyclodextrin ethanol solution is formed in 95% ethyl alcohol of 1mL;Beta-cyclodextrin ethanol solution is added in mixed liquor, in 50 DEG C, 2h is stirred under the conditions of 2000rpm, is filtered to obtain filtrate, distills 2h under the conditions of 50 DEG C, -0.1MPa, obtains the low not soap of 18g The antarctic krill oil of compound.
Through detecting, the content of unsaponifiable matter is in the low unsaponifiable matter antarctic krill oil that is prepared in this comparative example 1.05%, removal efficiency 54.3%, content of phospholipid 39.1%.
It is less to can be seen that manufacturing method step provided in the present invention compared with comparative example 1 through Examples 1 to 9, is made Reagent meets food safety specification, and the removal efficiency of unsaponifiable matter is higher, and content of phospholipid is higher, can be with large-scale application In industrial production.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (7)

1. a kind of preparation method of low unsaponifiable matter antarctic krill oil, which comprises the following steps:
S1. ethanol solution and mixed liquor, the concentration of the ethanol solution are uniformly mixing to obtain to slightly mentioning being added in antarctic krill oil It is 75~99%;
S2. the derivative of cyclodextrin and/or cyclodextrin is added into the mixed liquor, filtrate is stirred and be obtained by filtration, with described The total weight for slightly mentioning antarctic krill oil is 100% meter, the additional amount of the derivative of the cyclodextrin and/or cyclodextrin is 5~ 50%;
S3. vacuum distillation removing ethyl alcohol is carried out to the filtrate and obtains low unsaponifiable matter antarctic krill oil.
2. preparation method according to claim 1, wherein in step S2, the cyclodextrin is selected from beta-cyclodextrin, α-ring paste One of essence and gamma-cyclodextrin are a variety of, and the derivative of the cyclodextrin is selected from 2-HP-BETA-CD and 2,6- diformazan One of group-beta-cyclodextrin is a variety of.
3. preparation method according to claim 2, wherein described slightly to mention antarctic krill oil and 75~95% in step S1 Ethanol solution w/v be 1:(1~10).
4. preparation method according to claim 1, wherein in step S1, the condition of the stirring includes at -4~40 DEG C, 0.1~6h is stirred with 300~3000rpm.
5. preparation method according to claim 1, wherein in step S1, the condition of the stirring is included in 20~40 DEG C Under, 0.5~6h is stirred with 300~3000rpm.
6. preparation method according to claim 1, wherein in step S3, the condition of the vacuum distillation is 20~80 DEG C, -0.05~-0.1MPa distills 0.5~6h.
7. the low unsaponifiable matter antarctic krill oil that preparation method described according to claim 1~any one of 6 obtains.
CN201811290847.2A 2018-10-31 2018-10-31 A kind of low unsaponifiable matter antarctic krill oil and preparation method thereof Pending CN109181864A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107557138A (en) * 2017-11-01 2018-01-09 浙江海洋大学 A kind of method that ultrasound-assisted enzymolysis method prepares antarctic krill oil

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107557138A (en) * 2017-11-01 2018-01-09 浙江海洋大学 A kind of method that ultrasound-assisted enzymolysis method prepares antarctic krill oil

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
孙甜甜: "高品质南极磷虾虾油工业化生产技术研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
徐文思: "南极磷虾油的提取及精制工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

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Application publication date: 20190111