CN107874257A - The preparation method of high embedding rate small particle antarctic krill oil nanoparticle - Google Patents
The preparation method of high embedding rate small particle antarctic krill oil nanoparticle Download PDFInfo
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- CN107874257A CN107874257A CN201711096709.6A CN201711096709A CN107874257A CN 107874257 A CN107874257 A CN 107874257A CN 201711096709 A CN201711096709 A CN 201711096709A CN 107874257 A CN107874257 A CN 107874257A
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- antarctic krill
- krill oil
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 66
- 229940106134 krill oil Drugs 0.000 title claims abstract description 49
- 239000002245 particle Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000008346 aqueous phase Substances 0.000 claims abstract description 32
- 239000012071 phase Substances 0.000 claims abstract description 29
- 239000007908 nanoemulsion Substances 0.000 claims abstract description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003381 stabilizer Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 12
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims abstract description 12
- 239000000839 emulsion Substances 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 11
- 239000005018 casein Substances 0.000 claims abstract description 11
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000021240 caseins Nutrition 0.000 claims abstract description 11
- 239000011734 sodium Substances 0.000 claims abstract description 11
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 11
- 239000008363 phosphate buffer Substances 0.000 claims abstract description 7
- 239000012046 mixed solvent Substances 0.000 claims abstract description 3
- 235000015424 sodium Nutrition 0.000 claims description 10
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 9
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 9
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 235000020195 rice milk Nutrition 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000000877 morphologic effect Effects 0.000 abstract 1
- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 21
- 235000020673 eicosapentaenoic acid Nutrition 0.000 description 21
- 229960005135 eicosapentaenoic acid Drugs 0.000 description 21
- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000001514 detection method Methods 0.000 description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 8
- JEBFVOLFMLUKLF-IFPLVEIFSA-N Astaxanthin Natural products CC(=C/C=C/C(=C/C=C/C1=C(C)C(=O)C(O)CC1(C)C)/C)C=CC=C(/C)C=CC=C(/C)C=CC2=C(C)C(=O)C(O)CC2(C)C JEBFVOLFMLUKLF-IFPLVEIFSA-N 0.000 description 5
- 235000013793 astaxanthin Nutrition 0.000 description 5
- MQZIGYBFDRPAKN-ZWAPEEGVSA-N astaxanthin Chemical compound C([C@H](O)C(=O)C=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)C(=O)[C@@H](O)CC1(C)C MQZIGYBFDRPAKN-ZWAPEEGVSA-N 0.000 description 5
- 229940022405 astaxanthin Drugs 0.000 description 5
- 239000001168 astaxanthin Substances 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000003995 emulsifying agent Substances 0.000 description 5
- 238000000265 homogenisation Methods 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 210000000481 breast Anatomy 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000010812 external standard method Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 238000009777 vacuum freeze-drying Methods 0.000 description 4
- 241000238557 Decapoda Species 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 235000015067 sauces Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 229930182558 Sterol Natural products 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 235000003702 sterols Nutrition 0.000 description 2
- 150000003432 sterols Chemical class 0.000 description 2
- 241000239366 Euphausiacea Species 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- -1 glycerine Ester Chemical class 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 235000020660 omega-3 fatty acid Nutrition 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Mycology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Preparation And Processing Of Foods (AREA)
- Edible Oils And Fats (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention provides a kind of preparation method of high embedding rate small particle antarctic krill oil nanoparticle, concrete technical scheme is：Using the mixing of casein sodium, Arabic gum and polysorbas20 as stabilizer, phosphate buffer dissolving is added, produces aqueous phase；The in the mixed solvent that antarctic krill oil is dissolved in dichloromethane and acetone obtains oil phase；Oil phase is poured into aqueous phase, obtains thick nanoemulsions；Thick nanoemulsions are homogenized, be high-pressure homogeneous, the organic solvent in emulsion is finally removed under vacuum conditions, produces nano-emulsion；Obtained nano-emulsion is dried in vacuo, produces high embedding rate small particle antarctic krill oil nanoparticle.Circulating pressure of the invention by regulating and controlling emulsion high-pressure homogenizing process, the morphological homogeneity and embedding rate of antarctic krill oil nanoparticle are improved, reduce the grain size of nanoparticle.
Description
Technical field
The present invention relates to the preparation field of antarctic krill oil nanoparticle, and high homogeneity is prepared more specifically to one kind
And the preparation method of the antarctic krill oil nanoparticle of embedding rate, low nanoparticle particle diameter.
Background technology
Krill is the single living resources that quantity is maximum on the earth, and reserves are huge.Antarctic krill oil is mainly by glycerine
Ester, phosphatide, free fatty, sterol and astaxanthin composition.Antarctic krill oil is rich in phosphatide type Omega-3 polyunsaturated fatty acids
Its multiple biological activities is assigned with the characteristic of astaxanthin, but the oxidation stability of phosphatide type polyunsaturated fatty acid is significantly low
In the neutral grease such as glyceride and sterol；Free fatty has enzymatic oxidation effect, can reduce other and lipid components coexist
Oxidation stability, accelerate the deterioration of grease；And phosphatide water-swellable, cause poor solubility, influence its application in food.
In recent years, nanoparticle technology causes concern.Compared with common microcapsule, nanoparticle is except that can improve the thing that is embedded
Outside the physicochemical properties such as stability, dissolubility and decentralization, also in the absorption for increasing the thing that is embedded, the release for controlling the thing that is embedded etc.
Aspect shows the advantage of uniqueness.At present, prepare the method for nanoparticle have it is a variety of, such as：High pressure homogenization method, micro emulsion method, nanometer are sunk
Shallow lake method, emulsification mechanism etc..High pressure homogenization method is the method for preparing nanoparticle the most frequently used at present, and it is divided into the hot equal method of breast
With the cold equal method of breast, inevitably needing in the case of a high temperature to heat core and surfactant in preparation process makes its shape
Into molten condition, so that can be to such as astaxanthin of the heat-sensitive substance to containing in core, unrighted acid in preparation process
Etc. having an impact, make the reduction of its content.Equally, micro emulsion method needs to heat material during preparation, so as to reduce temperature-sensitive
The content of property material.Although nanoprecipitation method will not produce high temperature as nanoparticle preparation method in preparation process, making
Produce precipitation during standby, caused precipitation cannot pass through high-pressure homogeneous, and the particle diameter and homogeneity for causing nanoparticle can not obtain
Improve, and using less in reality produces.And for emulsification mechanism, then it is using solvent miscible with water as water
Phase, and with the immiscible organic solvent of water nanoscale emulsion droplet can be formed when aqueous phase contacts with oil phase, is then solidified as oil phase,
Isolated nanoparticle；Because it will not produce high temperature during preparation, obtain so that heat-sensitive substance can preferably retain,
The preparation of antarctic krill oil nanoparticle is accordingly can be applied to, the thermal sensitivity things such as astaxanthin and polyunsaturated fatty acid in shrimp sauce can be made
Matter preferably preserves.
Found by investigating early stage, forefathers are tentatively mixed to get thick breast during nanoparticle is prepared, by oil phase and aqueous phase
After agent, directly carried out under a certain pressure it is high-pressure homogeneous obtain nanoemulsions, particle diameter be present not in the nanoparticle for causing to be prepared
Homogeneous, the problems such as embedding rate is low, particle diameter is larger.
The content of the invention
In order to solve the above problems, the invention provides a kind of preparation of high embedding rate small particle antarctic krill oil nanoparticle
Method, including four steps such as the preparation of aqueous phase, the preparation of oil phase, high-pressure homogeneous and nanoparticle drying of emulsion, specific skill
Art scheme is：
S1, prepare aqueous phase：Raw material is mixed by following composition and percentage by weight, prepares aqueous phase：
Using the mixing of casein sodium, Arabic gum and Tween-20 as stabilizer, the stabilizer accounts for aqueous phase gross mass
1~3%, wherein, casein sodium accounts for the 60~70% of the stabilizer gross mass, and Arabic gum accounts for the total matter of the stabilizer
The 5~10% of amount, Tween-20 accounts for the 20~25% of the stabilizer gross mass；
The stabilizer is dissolved in pH=7 phosphate buffer, 0.5~2h is stirred at 20~70 DEG C, produces aqueous phase；
It is preferred that whipping temp is 40 DEG C~60 DEG C, mixing time is 0.5~1h；
Under preferred embodiment, the stabilizer accounts for the 2~3% of the aqueous phase gross mass, and casein sodium is made with Arabic gum
For the wall material of antarctic krill oil nanoparticle, Tween-20 is as emulsifying agent；When preparing aqueous phase, casein sodium and Arabic gum
Raised with the rise solubility of temperature, but Arabic gum viscosity decline with the rise of temperature, the present invention use certain
Temperature control step, ensure the viscosity of aqueous phase, control film forming situation；
Prepare oil phase：Antarctic krill oil is dissolved in the in the mixed solvent of dichloromethane and acetone, the dichloromethane with
The volume ratio of acetone is 1:(1~5), antarctic krill oil occupy 5~10 (g/100ml) of solvent；
Wherein, the volume ratio of dichloromethane and acetone preferably 1：(1~3)；
S2, oil phase made from step S1 is poured slowly into the aqueous phase, stirs 0.5~2h at 25 DEG C~45 DEG C, obtain
Thick nanoemulsions；The thick nanoemulsions are homogenized 5~10min under 6000~10000rpm/min rotating speeds；Then to emulsion
Carry out high-pressure homogeneous, sequentially carry out homogeneous under 0~50bar, 200~400bar, 550~650bar pressure, each 1 time, then
Homogeneous is circulated under 700~900bar pressure 3 times, finally remove the organic solvent in emulsion under vacuum conditions, produce nanometer
Breast；
Obtained nano-emulsion is dried in vacuo, produces high embedding rate small particle antarctic krill oil nanoparticle.
Wherein, the mixing time is preferably 1~1.5h.
The present invention is stirred using low temperature when mixing oil phase, avoids the heat-sensitive substance in shrimp sauce, such as astaxanthin, because
High temperature and the oxidative degradation occurred.
Under preferred embodiment, the thick nanoemulsions are homogenized 6~8min under 7000~8000rpm rotating speeds.
Under preferred embodiment, vacuum drying condition is described in step S2：
1~3h of pre-freeze at -60 DEG C~-50 DEG C；1~3h is kept at -45 DEG C~-40 DEG C, vacuum is extracted, makes its holding
1Par；1~3h is kept at -35 DEG C~-25 DEG C；4~8h is kept at -15 DEG C~-5 DEG C；4~8h of holding at 0 DEG C~-5 DEG C, 10 DEG C
4~8h is kept at~15 DEG C.The present invention uses gradient vacuum drying process, and shrimp sauce nanoparticle can be made preferably to keep original nanometer
Particle shape looks.
The technological innovation of the present invention is：
1st, the present invention is prepared antarctic krill oil nanoparticle and prepared based on emulsification mechanism, using multistage ladder
Degree circulation is high-pressure homogeneous, improves the homogeneity and embedding rate of antarctic krill oil nanoparticle, reduces antarctic krill oil nanoparticle
Particle diameter.Product dispersion index produced by the present invention drops to 0.302 from 0.659, the range of decrease 118%；Embedding rate rises from 61.83%
To 81.82%, amplification reaches 33.33%；Particle diameter drops to 132nm from 313nm, decreases by 137%.
2nd, method used in the present invention is simple and reliable, easy to operate, is circulated only with multistage gradient high-pressure homogeneous with regard to energy
Reach preferable effect.
To sum up, the inventive method improves antarctic krill oil nanoparticle homogeneity and embedding rate, reduces nanoparticle particle diameter,
Preparation method of the present invention by regulating and controlling the high-pressure homogeneous pressure in nanoparticle forming process, so as to improve the homogeneity of nanoparticle and
Embedding rate, reduce nanoparticle particle diameter.
Brief description of the drawings
Fig. 1 is high-pressure homogeneous to obtain the grain-size graph of nanoemulsions when being 0~50bar；
Fig. 2 is high-pressure homogeneous to obtain the grain-size graph of nanoemulsions when being 200~400bar；
Fig. 3 is high-pressure homogeneous to obtain the grain-size graph of nanoemulsions when being 550~650bar；
Fig. 4 is high-pressure homogeneous homogeneous 1 time under 0~50bar, 200~400bar and 550~650bar pressure, is then existed
Homogeneous is circulated under 700~900bar pressure and obtains the grain-size graph of nanoemulsions 3 times；
Fig. 5 is EPA standard curves.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1：
The preparation of thick emulsifying agent
0.3g antarctic krill oil is dissolved into 20ml dichloromethane and acetone soln, its ratio is 1：2, as oil
Phase.Stabilizer (casein sodium, Arabic gum and Tween-20) is dissolved into pH=7 phosphate buffer, stabilizer accounts for
The concentration of aqueous phase is 2%~3%, and it is 30 DEG C~60 DEG C that it, which adds temperature, 0.5~1h of mixing time.The mixing of oil phase and aqueous phase
Ratio is 1：9, oil phase is poured into aqueous phase, oil phase is mixed with water conjunction uniformly with magnetic agitation and refiner.
It is high-pressure homogeneous
Well mixed emulsion progress is high-pressure homogeneous, and its homogeneous power is 0~50bar circulation primaries.Then by nano-emulsion
Liquid carries out revolving and removes organic solvent under vacuum conditions.Obtained nanoemulsions carry out vacuum freeze drying, obtain nanoparticle.
The detection of particle diameter
It will be dissolved into by high-pressure homogeneous obtained nanoemulsions in deionized water, its ratio is 1；15~1：25.Pass through
Malvern laser particle analyzer is detected, as a result as shown in Figure 1.
The extraction of surface oil
The present invention will weigh 2~5g and freeze nanoparticle with conical flask, 30ml~50ml n-hexane then being added, 37
0.5h is extracted at DEG C, then collects supernatant, organic solvent is removed, so as to obtain surface oil.
The detection of embedding rate
The present invention detects antarctic krill oil nanoparticle bag using EPA (eicosapentaenoic acid) as standard items, by external standard method
Bury rate.EPA (eicosapentaenoic acid) standard curve (figure is obtained by GC-MS (6890N GC-5973 MSD Agilent) first
Shown in 5), the content of EPA in antarctic krill oil and antarctic krill oil nanoparticle surface oil is then calculated according to standard curve.South
The embedding rate of pole krill oil nanoparticle is measured by equation below：
The nanoparticle obtained according to above method, its particle diameter are 313.35 ± 19.12nm, and its dispersion index is 0.659, is surveyed
The embedding rate obtained is 61.83 ± 1.96%
Embodiment 2：
The preparation of thick emulsifying agent
0.3g antarctic krill oil is dissolved into 20ml dichloromethane and acetone soln, its ratio is 1：2, as oil
Phase.Stabilizer (casein sodium, Arabic gum and Tween-20) is dissolved into pH=7 phosphate buffer, stabilizer accounts for
The concentration of aqueous phase is 2%~3%, and it is 30 DEG C~60 DEG C that it, which adds temperature, 0.5~1h of mixing time.The mixing of oil phase and aqueous phase
Ratio is 1：9, oil phase is poured into aqueous phase, oil phase is mixed with water conjunction uniformly with magnetic agitation and refiner.
It is high-pressure homogeneous
Well mixed emulsion progress is high-pressure homogeneous, and its homogenization pressure is 200~400bar circulation primaries.Then will receive
Rice milk liquid carries out revolving and removes organic solvent under vacuum conditions.Obtained nanoemulsions carry out vacuum freeze drying, are received
The grain of rice.
The detection of particle diameter
It will be dissolved into by high-pressure homogeneous obtained nanoemulsions in deionized water, its ratio is 1；15~1：25.Pass through
Malvern laser particle analyzer is detected, as a result as shown in Figure 2.
The extraction of surface oil
The present invention will weigh 2~5g and freeze nanoparticle with conical flask, 30ml~50ml n-hexane then being added, 37
0.5h is extracted at DEG C, then collects supernatant, organic solvent is removed, so as to obtain surface oil.
The detection of embedding rate
The present invention detects antarctic krill oil nanoparticle bag using EPA (eicosapentaenoic acid) as standard items, by external standard method
Bury rate.EPA (eicosapentaenoic acid) standard curve (figure is obtained by GC-MS (6890N GC-5973 MSD Agilent) first
Shown in 5), the content of EPA in antarctic krill oil and antarctic krill oil nanoparticle surface oil is then calculated according to standard curve.South
The embedding rate of pole krill oil nanoparticle is measured by equation below：
The nanoparticle obtained according to above method, its particle diameter are 312.55 ± 16.07nm, and its dispersion index is 1, is measured
Embedding rate is 64.02 ± 1.43%.
Embodiment 3：
The preparation of thick emulsifying agent
0.3g antarctic krill oil is dissolved into 20ml dichloromethane and acetone soln, its ratio is 1：2, as oil
Phase.Stabilizer (casein sodium, Arabic gum and Tween-20) is dissolved into pH=7 phosphate buffer, stabilizer accounts for
The concentration of aqueous phase is 2%~3%, and it is 30 DEG C~60 DEG C that it, which adds temperature, 0.5~1h of mixing time.The mixing of oil phase and aqueous phase
Ratio is 1：9, oil phase is poured into aqueous phase, oil phase is mixed with water conjunction uniformly with magnetic agitation and refiner.
It is high-pressure homogeneous
Well mixed emulsion progress is high-pressure homogeneous, and its homogenization pressure is 550~650bar circulation primaries.Then will receive
Rice milk liquid carries out revolving and removes organic solvent under vacuum conditions.Obtained nanoemulsions carry out vacuum freeze drying, are received
The grain of rice.
The detection of particle diameter
It will be dissolved into by high-pressure homogeneous obtained nanoemulsions in deionized water, its ratio is 1；15~1：25.Pass through
Malvern laser particle analyzer is detected, as a result as shown in Figure 3.
The extraction of surface oil
The present invention will weigh 2~5g and freeze nanoparticle with conical flask, 30ml~50ml n-hexane then being added, 37
0.5h is extracted at DEG C, then collects supernatant, organic solvent is removed, so as to obtain surface oil.
The detection of embedding rate
The present invention detects antarctic krill oil nanoparticle bag using EPA (eicosapentaenoic acid) as standard items, by external standard method
Bury rate.EPA (eicosapentaenoic acid) standard curve (figure is obtained by GC-MS (6890N GC-5973 MSD Agilent) first
Shown in 5), the content of EPA in antarctic krill oil and antarctic krill oil nanoparticle surface oil is then calculated according to standard curve.South
The embedding rate of pole krill oil nanoparticle is measured by equation below：
The nanoparticle obtained according to above method, its particle diameter are 211.21 ± 6.59nm, and its dispersion index is 0.702, is surveyed
The embedding rate obtained is 75.43 ± 1.27%.
Embodiment 4：
The preparation of thick emulsifying agent
0.3g antarctic krill oil is dissolved into 20ml dichloromethane and acetone soln, its ratio is 1：2, as oil
Phase.
Stabilizer (casein sodium, Arabic gum and Tween-20) is dissolved into pH=7 phosphate buffer, surely
Determine agent account for aqueous phase concentration be 2%~3%, its add temperature be 30 DEG C~60 DEG C, 0.5~1h of mixing time.Oil phase and aqueous phase
Mixed proportion be 1：9, oil phase is poured into aqueous phase, oil phase is mixed with water conjunction uniformly with magnetic agitation and refiner.
It is high-pressure homogeneous
Well mixed emulsion is carried out high-pressure homogeneous, its homogenization pressure is 0~50bar, 200~400bar and 550~
Homogeneous 1 time under 650bar pressure, then circulates homogeneous 3 times under 700~900bar pressure.Then by nanoemulsions in vacuum shape
Revolving is carried out under state and removes organic solvent.Obtained nanoemulsions carry out vacuum freeze drying, obtain nanoparticle.
The detection of particle diameter
It will be dissolved into by high-pressure homogeneous obtained nanoemulsions in deionized water, its ratio is 1；15~1：25.Pass through
Malvern laser particle analyzer is detected, as a result as shown in Figure 4.
The extraction of surface oil
The present invention will weigh 2~5g and freeze nanoparticle with conical flask, 30ml~50ml n-hexane then being added, 37
Extracted at DEG C
0.5h, supernatant is then collected, organic solvent is removed, so as to obtain surface oil.
The detection of embedding rate
The present invention detects antarctic krill oil nanoparticle bag using EPA (eicosapentaenoic acid) as standard items, by external standard method
Bury rate.EPA (eicosapentaenoic acid) standard curve (figure is obtained by GC-MS (6890N GC-5973 MSD Agilent) first
Shown in 5), the content of EPA in antarctic krill oil and antarctic krill oil nanoparticle surface oil is then calculated according to standard curve.South
The embedding rate of pole krill oil nanoparticle is measured by equation below：
The nanoparticle obtained according to above method, its particle diameter are 130.93 ± 2.56nm, and its dispersion index is 0.302, is surveyed
The embedding rate obtained is 81.82 ± 1.35%
Table 1 is the particle diameter and embedding rate of nanoparticle under each high-pressure homogeneous pressure, by contrast it is different prepare it is high-pressure homogeneous
The particle diameter and embedding rate of the nanoemulsions of pressure, we can draw, the nanoparticle being prepared by the present invention can be effective
Reduction nanoparticle particle diameter, improve the homogeneity and embedding rate of nanoparticle.
Table 1：The particle diameter and embedding rate of nanoparticle under each high-pressure homogeneous pressure
Claims (6)
1. a kind of preparation method of high embedding rate small particle antarctic krill oil nanoparticle, it is characterised in that concrete technical scheme is：
S1, prepare aqueous phase：Raw material is mixed by following composition and percentage by weight, prepares aqueous phase：
Using the mixing of casein sodium, Arabic gum and Tween-20 as stabilizer, the stabilizer accounts for the 1 of aqueous phase gross mass
~3%, wherein, casein sodium accounts for the 60~70% of the stabilizer gross mass, and Arabic gum accounts for the stabilizer gross mass
5~10%, Tween-20 accounts for the 20~25% of the stabilizer gross mass；
The stabilizer is dissolved in pH=7 phosphate buffer, 0.5~2h is stirred at 20~70 DEG C, produces aqueous phase；
Prepare oil phase：Antarctic krill oil is dissolved in the in the mixed solvent of dichloromethane and acetone, the dichloromethane and acetone
Volume ratio be 1:(1~5), antarctic krill oil occupy 5~10 (g/100ml) of solvent；
S2, oil phase made from step S1 is poured slowly into the aqueous phase, stirs 0.5~2h at 25 DEG C~45 DEG C, slightly received
Rice milk liquid；The thick nanoemulsions are homogenized 5~10min under 6000~10000rpm/min rotating speeds；Then emulsion is carried out
It is high-pressure homogeneous, homogeneous 1 time is distinguished under 0~50bar, 200~400bar, 550~650bar pressure, then 700~
Homogeneous is circulated under 900bar pressure 3 times, finally remove the organic solvent in emulsion under vacuum conditions, produce nano-emulsion；
Obtained nano-emulsion is dried in vacuo, produces high embedding rate small particle antarctic krill oil nanoparticle.
2. the preparation method of high embedding rate small particle antarctic krill oil nanoparticle according to claim 1, it is characterised in that step
Stabilizer described in rapid S1 accounts for the 2~3% of the aqueous phase gross mass.
3. the preparation method of high embedding rate small particle antarctic krill oil nanoparticle according to claim 1, it is characterised in that step
It is 40 DEG C~60 DEG C that rapid S1, which prepares whipping temp described in aqueous phase, and mixing time is 0.5~1h.
4. the preparation method of high embedding rate small particle antarctic krill oil nanoparticle according to claim 1, it is characterised in that step
It is 1 that rapid S1, which prepares oil phase dichloromethane and the volume ratio of acetone,：(1~3).
5. the preparation method of high embedding rate small particle antarctic krill oil nanoparticle according to claim 1, it is characterised in that step
Rapid S2 mixings time are 1~1.5h；The thick nanoemulsions are homogenized 6~8min under 7000~8000rpm rotating speeds.
6. the preparation method of high embedding rate small particle antarctic krill oil nanoparticle according to claim 1, it is characterised in that step
Suddenly vacuum drying condition described in S2 is：
1~3h of pre-freeze at -60 DEG C~-50 DEG C；1~3h is kept at -45 DEG C~-40 DEG C, extracts vacuum, it is kept 1Par；-35
DEG C~-25 DEG C at keep 1~3h；4~8h is kept at -15 DEG C~-5 DEG C；4~8h is kept at 0 DEG C~-5 DEG C, at 10 DEG C~15 DEG C
Keep 4~8h.
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