CN110338235A - A kind of preparation process loading flax oil nano emulsions - Google Patents
A kind of preparation process loading flax oil nano emulsions Download PDFInfo
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- CN110338235A CN110338235A CN201910592866.9A CN201910592866A CN110338235A CN 110338235 A CN110338235 A CN 110338235A CN 201910592866 A CN201910592866 A CN 201910592866A CN 110338235 A CN110338235 A CN 110338235A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/06—Preservation of finished products
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Abstract
The invention discloses a kind of preparation process for loading flax oil nano emulsions, which includes: to mix starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, and wall material is obtained after standing and mixes aqueous solution；The mass ratio of the starch Sodium Octenyl Succinate and soybean protein isolate is 1:0.5~6；Linseed oil is instilled the wall material to mix in aqueous solution, is pre-mixed under conditions of magnetic agitation, thick lotion is obtained；The linseed oil and the mass ratio of wall material phase are 1:0.2~5；Using thick lotion described in ultrasonication, the nanoemulsions of load linseed oil are obtained.Preparation process of the present invention is obtained to load flax oil nano emulsions, not only partial size is small, embedding rate is high, and it being capable of effective blocking oxygen, slow down the oxygen speed of action, the stability for enhancing nanoemulsions, retains the nutritional ingredient of linseed oil, improves the water solubility of linseed oil, its application range is widened simultaneously, increases its bioavilability.
Description
Technical field
The present invention relates to edible flax oil nano emulsions preparation technical field more particularly to a kind of load linseed oil nanometers
The preparation process of lotion.
Background technique
Flax belongs to traditional oil crops in China, and oil seed flax oil-containing is generally 40~60%, wherein there are many containing
Unsaturated fatty acid, such as alpha-linolenic acid, linoleic acid, oleic acid etc., wherein most important fatty acid is linolenic acid, content about 50% is left
The right side, platymiscium oil most.Linolenic acid belongs to ω -3 series fatty acid, studies have shown that ω -3 series fatty acid has the U.S. in human body
13 kinds of physiological functions that FDA is announced, as adjusted the formation and development mechanism of atherosclerosis, reducing cardiovascular disease generation
Probability, promotion intellectual development, adjusting immune system, reduction blood lipid, inhibition malignant tumour etc..
Go bad since linseed oil is oxidizable during production and processing, storage and culinary art etc., especially alpha-linolenic acid structure
In three double bonds be easy to oxidation, it is rancid, cause smell bad, linseed oil per se with special odor it is also heavier, liquid
State is also difficult to be added in daily bread, and then influences its application.To overcome the above disadvantages, it is necessary to have to linseed oil
Effect embedding.A large amount of Science Explorations, which shows to be remarkably reinforced through method of modifying such as emulsification, embedding, loads, plants the water-soluble of linseed oil
Property and its special odor can be covered, and retain its original nutriment, it made to be applied to more areas.
In research so far, linseed oil has been fully applicable to friction resistance material, plasticizer, health food, animal
The fields such as feed, pharmaceutical synthesis.Since linseed oil is natural materials, itself is non-toxic, and extraction process is mature and safety, pass through by
Its nanoemulsions that load linseed oil is made, improves its application effect while increasing its application range.
Supersound method is mutually to be uniformly mixed with water phase using the ultrasonic wave of sufficiently large acoustic pressure by oily, forms dispersion system.
The main function mechanism of ultrasonic emulsification is cavitation effect.When the sufficiently large acoustic irradiation liquid of frequency, can make between liquid phase molecule
Attraction be broken within the loose half period, formed cavitation bubble, cavitation bubble is under sound wave positive pressure phase separation, and volume is extremely short
Times compression, occurs stable cavitation or transient cavitation in time.Wherein, the cavitation bubble that transient cavitation occurs deforms to heavens, occurs
Rupture, generates instantaneous localized hyperthermia and high pressure, and this effect then will lead to oil droplet rupture, complete emulsification, and influence a nanometer model
Enclose interior partial size.
Summary of the invention
The present invention is directed to linseed oil encapsulated product partial size in the prior art and contains greatly, in the alpha-linolenic acid structure of linseed oil
Three double bonds be easy to oxidation, it is rancid, and cause alpha-linolenic acid oxidation, it is rancid after taste by extreme influence, product product
The problems such as matter changes, and influences product storage, reduces the actual use value of linseed oil, provides a kind of load linseed oil and receives
The preparation process of rice milk liquid, load flax oil nano emulsions of technique preparation, not only partial size is small, embedding rate is high, but also can
Effective blocking oxygen slows down the oxygen speed of action, enhances the stability of nanoemulsions, retains the nutritional ingredient of linseed oil, improves
The water solubility of linseed oil, while its application range is widened, increase its bioavilability.
Specific technical solution is as follows:
A kind of preparation process loading flax oil nano emulsions, comprising the following steps:
(1) it mixes starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, wall material is obtained after standing
Mix aqueous solution；
The mass ratio of the starch Sodium Octenyl Succinate and soybean protein isolate is 1:0.5~6；
(2) linseed oil is instilled the wall material to mix in aqueous solution, is pre-mixed, is obtained under conditions of magnetic agitation
To thick lotion；
The linseed oil and the mass ratio of wall material phase are 1:0.2~5；
(3) using thick lotion described in ultrasonication, the nanoemulsions of load linseed oil are obtained.
Innovation of the invention is: by the starch Sodium Octenyl Succinate and soybean protein isolate of specific usage ratio
It is combined as wall material, embeds linseed oil, obtain the nanoemulsions of load linseed oil；On the one hand pass through reasonable preparation process
The nanoemulsions product that partial size is small, embedding rate is high and barodynamics is stable is obtained with raw material dosage ratio；On the other hand, soybean is utilized
Starch Sodium Octenyl Succinate, which is added, in protein isolate to form one layer of hydration shell in oil-water interfaces, thus effective blocking oxygen,
The oxidation rate for slowing down linseed oil (three double bonds in alpha-linolenic acid) improves the stability of nanoemulsions, retains flax
The nutritional ingredient of oil, improves the water solubility of linseed oil, while widening its application range, increases its bioavilability.In addition, above-mentioned
The nanoemulsions that preparation process obtains are by freeze-drying or are spray-dried available linseed oil embedded nano particle.
Preferably, the mass ratio of the starch Sodium Octenyl Succinate and soybean protein isolate is 1:2 in step (1)
~6；It is further preferred that the mass ratio is 1:2.
Preferably, the mass ratio of the linseed oil and wall material phase is 1:0.2~1.5 in step (2).
Preferably, in step (1), the wall material mix the mass concentration of wall material phase in aqueous solution be 1%~
1.5%；Whipping temp when mixing is 40~50 DEG C, 3~5h of Shi Changwei.
Preferably, the mass ratio of the linseed oil and wall material phase is 1:1.5 in step (1).
It is further preferred that the mass ratio of the starch Sodium Octenyl Succinate and soybean protein isolate is 1:2, and the linseed oil
Mass ratio with wall material phase is 1:1.5.
Preferably, the temperature of the magnetic agitation is 10~40 DEG C in step (2), the revolving speed of magnetic agitation is 1000
~1500r/min, when a length of 10min~40min of magnetic agitation.
It is further preferred that the temperature of the magnetic agitation is 25 DEG C, the revolving speed of magnetic agitation is 1300r/min, magnetic agitation
Shi Changwei 15min.
Preferably, the energy density of the ultrasonication is 7200~10800J/mL in step (3).It is sent out through experiment
Existing, the ultrasound energy density of input is 10800J/mL, and emulsion particle diameter is minimum.
Preferably, in step (3), the condition of the ultrasonication are as follows: frequency is 20~30KHz, power is 400~
600W.Ultrasonic procedure uses ice-water bath.
Preferably, in step (3), during ultrasonication, using lasting or interval ultrasound mode, ultrasonic time
For 10~25min.
It is further preferred that using power for the ultrasonication (i.e. ultrasonic wave added) of 600W in step (3), the arteries and veins of " 8s " is selected
Rush mode, ultrasonic time 20min.
It further, further include step (4), specifically: the nanoemulsions of linseed oil are loaded described in step (3) through cold
After dry or spray drying treatment is lyophilized, nano particle is obtained.
The present invention also provides flax oil nano emulsions are loaded made from the preparation process.
Compared with prior art, the invention has the following advantages:
(1) starch Sodium Octenyl Succinate of specific usage ratio and soybean protein isolate are combined by the method for the present invention
As wall material, linseed oil is embedded, obtains the nanoemulsions of load linseed oil；Not only partial size is small, embedding rate is high, again for the nanoemulsions
Mechanics stablize, and can effective blocking oxygen, slow down the oxidation rate of linseed oil, improve the stability of nanoemulsions,
The nutritional ingredient for retaining linseed oil, improves the water solubility of linseed oil, while widening its application range, increases its bioavilability.
(2) the method for the present invention obtains nanoemulsions by ultrasonic emulsification, and not only preparation process time-consuming is short, high-efficient,
And the property that the lotion obtained has barodynamics stable, and partial size is small, average grain diameter is 246.83 ± 4.49nm.
Detailed description of the invention
Fig. 1 is the influence of embodiment 1, embodiment 2 and 3 preparation method of comparative example to nanoemulsions particle size.
Fig. 2 is embodiment 1, nanoemulsions and bulk oil, independent soybean separation protein made from embodiment 2 and comparative example 3
The dsc analysis result of white raw material, independent starch Sodium Octenyl Succinate raw material.
Fig. 3 is that the FTIR of embodiment 1, embodiment 2, comparative example 3 and bulk oil analyzes result.
Specific embodiment
The invention will be further described combined with specific embodiments below, and what is be exemplified below is only specific implementation of the invention
Example, but protection scope of the present invention is not limited only to this.The present invention is further explained combined with specific embodiments below, the present invention
Implemented according to inventive technique scheme, gives detailed embodiment and operating procedure, but protection scope of the present invention is simultaneously
It is not limited to the following embodiments.
In the following examples, the experimental methods for specific conditions are not specified, usually according to normal condition；Involved by the following example
And each specific assay method is as follows:
(1) ultrasonic energy density
Calculation formula:
(2) accelerated oxidation is tested:
50ml sample liquid is put into the dark bottles of sealing 6 days, and is incubated in forced ventilation baking oven in 65 DEG C, wherein 1
Its expression stores about 1 month at room temperature.Remove processed sample after 0,1,3 and 6 day and measure oxygenation parameters (PV,
TBARS), specific requirement is as follows:
A) measurement of PV value: by the samples of latex (300 μ L) after accelerated oxidation, with 1.5mL isooctane/aqueous isopropanol
(3:2, v/v) mixing, obtaining final volume is 1.80mL.Mixture is vortexed three times, it is for 10 seconds every time, and be centrifuged
(3400g, 5min).Then, 200 μ L upper organic phases are added in 2.8mL chloroform/methanol (7:3, v/v) solution, then plus
Enter the ammonium thiocyanate solution (3.94mol/L) and 15 μ LFe of 15 μ L2+Solution (0.072mol/L, 1.5mL 0.144mol/L
FeSO4With 1.5mL0.132mol/L BaCl2Obtained in the supernatant that solution is mixed to get in 0.4mol/L hydrochloric acid), be vortexed vibration
It swings 4 seconds and is protected from light standing at room temperature 20 minutes, then read using the absorbance that UV spectrophotometer measures sample at 500nm
Number.
Use Fe3+Standard curve (using μ g/mL) measurement lipid hydroperoxide concentration.Peroxide value (PV) is expressed as every kilogram
The milliequivalent of peroxide in sample:
PV=(AS-ASB-ARB)/[(m×55.84×m0×2)×4.5]
Wherein, ASIt is the absorbance of sample；ASBIt is the absorbance of blank sample；ARBIt is the absorbance of blank reagent；M is from school
The slope that directrix curve obtains；M0 is the quality of oil in grams；55.84 be the atomic weight of iron, and 2 be to indicate peroxide number
Necessary splitting factor, rather than millinormal oxygen；4.5 are equivalent to the inverse of dilution gfactor relevant to isooctane organic phase
(0.9/0.2)。
B) measurement of TBARS value: 0.1mL lotion is mixed in test tube with 0.9mL water and 2mL TBA reagent, is placed in
15min in boiling water bath.Pipe is cooled to room temperature 10min, is then centrifuged for (12000rpm, 15min), supernatant is collected, use is ultraviolet
Visible spectrophotometer measures the absorbance at wavelength 532nm.According to the song of the standard made of 1,1,3,3- tetraethoxypropane
Line measures the content of MDA (malonaldehyde) in sample.
Embodiment 1
A kind of preparation process loading flax oil nano emulsions, the specific steps are as follows:
(1) it mixes starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, wall material is obtained after standing
Mix aqueous solution；
Taking 50mL mass concentration is that 1.25% wall material mixes aqueous solution；Wherein, ocentyl succinic is separated with soybean
The mass ratio of albumen is 1:2 (that is: soybean protein isolate accounting in wall material phase is 2/3)；
(2) be added dropwise into mixed aqueous solution 0.4167g linseed oil (that is: the mass ratio of linseed oil and wall material phase is 1:
1.5), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring, obtain thick lotion；
(3) under conditions of ultrasonic energy density is 7200J/mL, ultrasonication is carried out to thick lotion, preparation load is sub-
The nanoemulsions of sesame oil；
The condition of ultrasonication are as follows: FS-1200pv probe type ultrasonic processor, supersonic frequency 20KHz, power are
600W, mixed process select " 8s " ultrasound mode, ultrasonic time 20min.
(4) nanoemulsions of preparation are obtained into linseed oil nano particle by freeze-drying.
Embodiment 2
A kind of preparation process loading flax oil nano emulsions, the specific steps are as follows:
(1) it mixes starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, after standing, obtains wall material
Mix aqueous solution；
Taking 50mL mass concentration is that 1.25% wall material mixes aqueous solution；Wherein, ocentyl succinic is separated with soybean
The mass ratio of albumen is 1:0.5 (that is: soybean protein isolate accounting in wall material phase is 1/3)；
(2) be added dropwise into mixed aqueous solution 0.4167g linseed oil (that is: the mass ratio of linseed oil and wall material phase is 1:
1.5), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring, obtain thick lotion；
(3) under conditions of ultrasonic energy density is 7200J/mL, ultrasonication is carried out to thick lotion, preparation load is sub-
The nanoemulsions of sesame oil；
The condition of ultrasonication are as follows: FS-1200pv probe type ultrasonic processor, supersonic frequency 20KHz, power are
600W, mixed process select " 8s " ultrasound mode, ultrasonic time 20min.
(4) nanoemulsions of preparation are obtained into embedding linseed oil nano particle by spray drying.
Embodiment 3
A kind of preparation process loading flax oil nano emulsions, the specific steps are as follows:
(1) it mixes starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, wall material is obtained after standing
Mix aqueous solution；
Taking 50mL mass concentration is that 1.25% wall material mixes aqueous solution；Wherein, ocentyl succinic is separated with soybean
The mass ratio of albumen is 1:6 (that is: soybean protein isolate accounting in wall material phase is 6/7)；
(2) be added dropwise into mixed aqueous solution 0.4167g linseed oil (that is: the mass ratio of linseed oil and wall material phase is 1:
1.5), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring, obtain thick lotion；
(3) under conditions of ultrasonic energy density is 7200J/mL, ultrasonication is carried out to thick lotion, preparation load is sub-
The nanoemulsions of sesame oil；
The condition of ultrasonication are as follows: FS-1200pv probe type ultrasonic processor, supersonic frequency 20KHz, power are
600W, mixed process select " 8s " ultrasound mode, ultrasonic time 20min.
(4) nanoemulsions of preparation are obtained into embedding linseed oil nano particle by freeze-drying.Comparative example 1
The mass ratio of ocentyl succinic and soybean protein isolate is that (that is: soybean protein isolate exists 1:0.2 in this comparative example
Accounting is 1/6) outside, remaining content is identical with embodiment 1 in wall material phase.
Specific step is as follows:
(1) it mixes starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, wall material is obtained after standing
Mix aqueous solution；
Taking 50mL mass concentration is that 1.25% wall material mixes aqueous solution；Wherein, ocentyl succinic is separated with soybean
The mass ratio of albumen is 1:0.2 (that is: soybean protein isolate accounting in wall material phase is 1/6)；
(2) be added dropwise into mixed aqueous solution 0.4167g linseed oil (that is: the mass ratio of linseed oil and wall material phase is 1:
1.5), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring, obtain thick lotion；
(3) under conditions of ultrasonic energy density is 7200J/mL, ultrasonication is carried out to thick lotion, preparation load is sub-
The nanoemulsions of sesame oil；
The condition of ultrasonication are as follows: FS-1200pv probe type ultrasonic processor, supersonic frequency 20KHz, power are
600W, mixed process select " 8s " ultrasound mode, ultrasonic time 20min.
(4) nanoemulsions of preparation are obtained into embedding linseed oil nano particle by freeze-drying.
Comparative example 2
The mass ratio of ocentyl succinic and soybean protein isolate is that (that is: soybean protein isolate exists 1:10 in this comparative example
Accounting is 10/11) outside, remaining content is identical with embodiment 1 in wall material phase.
Specific step is as follows:
(1) it mixes starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, wall material is obtained after standing
Mix aqueous solution；
Taking 50mL mass concentration is that 1.25% wall material mixes aqueous solution；Wherein, ocentyl succinic is separated with soybean
The mass ratio of albumen is 1:10 (that is: soybean protein isolate accounting in wall material phase is 10/11)；
(2) be added dropwise into mixed aqueous solution 0.4167g linseed oil (that is: the mass ratio of linseed oil and wall material phase is 1:
1.5), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring, obtain thick lotion；
(3) under conditions of ultrasonic energy density is 7200J/mL, ultrasonication is carried out to thick lotion, preparation load is sub-
The nanoemulsions of sesame oil；
The condition of ultrasonication are as follows: FS-1200pv probe type ultrasonic processor, supersonic frequency 20KHz, power are
600W, mixed process select " 8s " ultrasound mode, ultrasonic time 20min.
Embodiment 4
The present embodiment is in addition to the mass ratio of core material linseed oil and wall material phase is 1:0.2, i.e., in the wall material phase of 50mL 1.25%
The linseed oil of 0.125g is added dropwise, remaining is identical with embodiment 1.
Embodiment 5
The present embodiment drips in addition to the mass ratio of core material linseed oil and wall material phase is 1:5 in the wall material phase of 50mL 1.25%
Add the linseed oil of 3.125g, remaining is identical with embodiment 1.
Comparative example 3
Only with starch Sodium Octenyl Succinate as wall material in this comparative example, remaining content is identical with embodiment 1.
Specific step is as follows:
(1) it mixes starch Sodium Octenyl Succinate is soluble in water, starch Sodium Octenyl Succinate is obtained after standing
Wall material aqueous solution；
Taking 50mL mass concentration is 1.25% starch Sodium Octenyl Succinate wall material aqueous solution；
(2) linseed oil (that is: the linseed oil and wall of 0.4167g are added dropwise into starch Sodium Octenyl Succinate wall material aqueous solution
The mass ratio of material phase is 1:1.5), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring,
Obtain thick lotion；
(3) under conditions of ultrasonic energy density is 7200J/mL, ultrasonication is carried out to thick lotion, preparation load is sub-
The nanoemulsions of sesame oil；
The condition of ultrasonication are as follows: FS-1200pv probe type ultrasonic processor, supersonic frequency 20KHz, power are
600W, mixed process select " 8s " ultrasound mode, ultrasonic time 20min.
(4) nanoemulsions of preparation are obtained into embedding linseed oil nano particle by freeze-drying.
Comparative example 4
In this comparative example in addition to core material linseed oil and the mass ratio of wall material starch Sodium Octenyl Succinate are 1:0.2, remaining
Content is identical with comparative example 3.
Specific step is as follows:
(1) it mixes starch Sodium Octenyl Succinate is soluble in water, starch Sodium Octenyl Succinate is obtained after standing
Wall material aqueous solution；
Taking 50mL mass concentration is 1.25% starch Sodium Octenyl Succinate wall material aqueous solution；
(2) linseed oil (that is: the linseed oil and wall material of 3.125g are added dropwise into starch Sodium Octenyl Succinate wall material aqueous solution
The mass ratio of phase is 1:0.2), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring, are obtained
To thick lotion；
(3) under conditions of ultrasonic energy density is 7200J/mL, ultrasonication is carried out to thick lotion, preparation load is sub-
The nanoemulsions of sesame oil；
The condition of ultrasonication are as follows: FS-1200pv probe type ultrasonic processor, supersonic frequency 20KHz, power are
600W, mixed process select " 8s " ultrasound mode, ultrasonic time 20min.
Comparative example 5
Except step (3) use high speed dispersion unit style for nanoemulsions, remaining step and 3 phase of comparative example in this comparative example
Together.
Specific step is as follows:
(1) it mixes starch Sodium Octenyl Succinate is soluble in water, starch Sodium Octenyl Succinate is obtained after standing
Wall material aqueous solution；
Taking 50mL mass concentration is 1.25% starch Sodium Octenyl Succinate wall material aqueous solution；
(2) linseed oil (that is: the linseed oil and wall of 0.4167g are added dropwise into starch Sodium Octenyl Succinate wall material aqueous solution
The mass ratio of material phase is 1:1.5), at 25 DEG C, the revolving speed of magnetic agitation 15min, stirring are 1300r/min, after stirring,
Obtain thick lotion；
(3) high speed shear processing is carried out to thick lotion using high speed dispersion unit (T18 basic model dispersion machine), prepares nanometer
Lotion；
The condition of high speed shear processing are as follows: (20000rpm) high speed shear 4min under intense mixing conditions.
The detection of nanoemulsions product property:
1, embedding rate, partial size and Zeta potential
It takes nanoemulsions made from 15mL above-described embodiment 1~5 and comparative example 1~5 to be put into sample bottle and carries out standing observation,
And carry out the measurement (Omni dynamic light scattering partial size and Zeta potential analyzer) of partial size and Zeta potential.As a result such as table 1 and Fig. 1
It is shown.
| Case | Embedding rate (%) | Partial size (nm) | Zeta potential (mV) |
| Embodiment 1 | 74.56±4.20 | 246.83±4.49 | -69.28±3.99 |
| Embodiment 2 | 75.14±4.94 | 243.96±3.03 | -67.21±2.98 |
| Embodiment 3 | 76.12±3.18 | 260.23±5.03 | -62.35±1.48 |
| Embodiment 4 | 80.12±1.19 | 250.43±3.43 | -68.13±2.97 |
| Embodiment 5 | 20.12±5.29 | 280.12±5.63 | -62.12±6.97 |
| Comparative example 1 | 78.16±2.81 | 230.77±3.32 | -43.25±1.74 |
| Comparative example 2 | / | >1000 | / |
| Comparative example 3 | 79.16±0.83 | 218.11±3.90 | -38.22±0.28 |
| Comparative example 4 | 25.23±0.33 | 185.14±4.57 | -38.24±0.28 |
| Comparative example 5 | / | >1000 | / |
As shown in Table 1, linseed oil and the addition mass ratio of wall material phase are 1:1.5, wherein starch Sodium Octenyl Succinate and
The mass ratio of soybean protein isolate is 1:2, using supercritical ultrasonics technology, and when to input ultrasonic energy density be 7200J/mL, nano-emulsion
Liquid is most stable, and its partial size is smaller, and Zeta potential absolute value is larger.
2, dsc analysis
Dsc analysis method is as follows:
The nanoemulsions of preparation are obtained into linseed oil nano particle by freeze-drying or spray drying.
Using Q20 differential scanning calorimeter, about 5~10mg sample is weighed in aluminum cup, using punching press pond to its into
Row sealing, is put into calorimetric pond.After setting temperature program, it is measured.Operating parameter: temperature elevating range is 25 DEG C~250 DEG C；Heating
Rate is 10 DEG C/min；Nitrogen flow is 50mL/min.
As a result as shown in Figure 1, in embodiment 1,2 and comparative example 3, the melting characteristic of SPI and SSOS itself by all or
Part is covered, and illustrates that both SPI and SSOS are compatible, and the melting peak area of lotion is smaller, shows good thermostabilization
Property, illustrate that the combination of SPI and SSOS play the role of stable emulsion.
3, FTIR is analyzed
FTIR analysis method is as follows:
The nanoemulsions of preparation are obtained into linseed oil nano particle by freeze-drying or spray drying.Utilize KBr tabletting
Method characterizes the functional group of sample.Take dry potassium bromide and quality be the centesimal solid sample to be tested of potassium bromide in
It is uniformly mixed in agate alms bowl, it is sufficiently levigate, it is pressed into thin slice (diameter 13mm, the diascope of thickness about 1mm).If being liquid to test sample
Body after then taking a small amount of potassium bromide to grind and be pressed into thin slice, uniformly drips upper drop sample to be tested on surface and is measured.Spectral region
Select 4000cm-1~600cm-1, resolution ratio selection 4cm-1Lower scanning 32 times.
As a result as shown in Fig. 2, 3400cm-1Place is H2The stretching vibration of O hydroxyl, 1020cm-1Place is the characteristic peak of SSOS,
The response of transmitance meets the increase and decrease of contained SSOS ratio in three kinds of nano particles (embodiment 1, embodiment 2 and comparative example 3)
Rule.
1657cm-1And 1547cm-1Place corresponds to amide I, II band, is the characteristic peak of protein, 1750cm-1Place is ester group
Existing proof, the absorption peak of linseed oil is maximum herein, and the response of excess-three sample is respectively less than the peak of linseed oil, illustrates cream
The embedding of liquid works well；710cm-1The absorption peak at place is related with double bond, it is observed here that nano particle (embodiment 1, it is real
Apply example 2 and comparative example 3) absorption peak be significantly less than the absorption peak of linseed oil, illustrate that the embedding of lotion works well.
4, accelerated oxidation is tested
To nanoemulsions made from Examples 1 to 3 and comparative example 1 and 3 carry out accelerated oxidation experiment, measurement PV value and
TBARS value, as a result as shown in table 2, table 3 and figure.
The PV value of nanoemulsions made from the different embodiments of table 2 and bulk oil
| Case | 0th day | 1st day | 3rd day | 6th day |
| Embodiment 1 | 0.1226±0.0084a | 0.5744±0.0276b | 0.7363±0.0244c | 1.0743±0.0215d |
| Embodiment 2 | 0.0157±0.0045a | 1.2986±0.0594bc | 1.4397±0.1582c | 1.1331±0.1167b |
| Embodiment 3 | 0.0187±0.0045a | 0.3721±0.0177b | 0.5373±0.0214c | 1.0123±0.0115d |
| Comparative example 1 | 0.1233±0.0122a | 2.1543±0.0232d | 1.7532±0.0331c | 0.8532±0.0541b |
| Comparative example 3 | 0.2911±0.0383a | 5.1037±0.1185c | 7.7187±0.4659d | 0.7875±0.0250b |
| Bulk oil | 0.0263±0.0091a | 1.9935±0.0454d | 1.6848±0.0333c | 0.6929±0.0314b |
Unit: mg/Kg oil.There were significant differences (p < 0.05, n=3) for different Superscript letters representative in colleague.
As shown in Table 2, the PV value fluctuation of 3 nanoemulsions of comparative example is most violent, reaches peak value in the third day of accelerated oxidation,
Much higher than the PV value of oil samples in bulk on the same day, illustrate only there is the work for promoting to aoxidize by wall material of starch Sodium Octenyl Succinate
With.PV value and bulk oil is close in comparative example 1, illustrates that the mass ratio of ocentyl succinic and soybean protein isolate is 1:0.2
When, nanoemulsions are weaker to the oxidation obstructing capacity of linseed oil；During accelerated oxidation, the PV value of embodiment 1,2,3 is close to be dissipated
The PV value of charge of oil, and the 6th day PV value of embodiment 2 is still below highest PV value in bulk oil 6 days, illustrates to be added in wall material
Soybean protein isolate, which mixes wall material, can play the role of slowing down oxidation rate.
The TBARS value of nanoemulsions made from the different embodiments of table 3 and bulk oil
| Case | 0th day | 1st day | 3rd day | 6th day |
| Embodiment 1 | 1.1736±0.2747a | 1.8080±0.2379a | 2.5216±0.4758ab | 4.0283±2.0784b |
| Embodiment 2 | -1.7511±0.0000a | 2.9817±0.2366c | 2.6661±0.7229bc | 1.7196±0.6831b |
| Embodiment 3 | 1.0214±0.1743a | 1.1120±0.0369a | 1.9217±0.3761ab | 3.2890±1.8794b |
| Comparative example 1 | 1.2378±0.3667a | 21.6812±6.5325b | 28.8714±4.1355c | 20.3467±3.5521b |
| Comparative example 3 | 1.4137±0.4960a | 37.3911±9.5135c | 41.8386±9.6164c | 17.4566±0.8367b |
| Bulk oil | -0.3336±0.2383a | 3.3996±1.5133b | 4.4322±0.4127bc | 5.7031±0.1376c |
Unit: mmolMAD/Kg oil.There were significant differences (p < 0.05, n=3) for different Superscript letters representative in colleague.
As shown in Table 3, the TBARS value fluctuation of 3 nanoemulsions of comparative example is most obvious, reaches peak in the third day of accelerated oxidation
Value illustrates that 3 wall material of comparative example plays the role of promoting oxidation, this is obtained with table 2 much higher than the TBARS value of oil samples in bulk on the same day
The conclusion arrived is consistent.TBARS value is higher than bulk oil in comparative example 1, is lower than comparative example 3, illustrates ocentyl succinic and soybean point
When mass ratio from albumen is 1:0.2, nanoemulsions are weaker to the oxidation obstructing capacity of linseed oil；Generating secondary oxidation product
Stage, the TBARS value of embodiment 1,2,3 is below comparative example 3, and oxidation can effectively be slowed down by showing preferred mixing wall material
Effect.
Claims (9)
1. a kind of preparation process for loading flax oil nano emulsions, which comprises the following steps:
(1) it mixes starch Sodium Octenyl Succinate and soybean protein isolate are soluble in water, wall material is obtained after standing and is mutually mixed
Heshui solution；
The mass ratio of the starch Sodium Octenyl Succinate and soybean protein isolate is 1:0.5~6；
(2) linseed oil is instilled the wall material to mix in aqueous solution, is pre-mixed under conditions of magnetic agitation, obtained thick
Lotion；
The linseed oil and the mass ratio of wall material phase are 1:0.2~5；
(3) using thick lotion described in ultrasonication, the nanoemulsions of load linseed oil are obtained.
2. the preparation process of load flax oil nano emulsions as described in claim 1, which is characterized in that described in step (1)
The mass ratio of starch Sodium Octenyl Succinate and soybean protein isolate is 1:2~6.
3. the preparation process of load flax oil nano emulsions as described in claim 1, which is characterized in that described in step (2)
Linseed oil and the mass ratio of wall material phase are 1:0.2~1.5.
4. the preparation process of load flax oil nano emulsions as described in claim 1, which is characterized in that described in step (2)
The temperature of magnetic agitation is 10~40 DEG C, and the revolving speed of magnetic agitation is 1000~1500r/min, magnetic agitation when it is a length of
10min~40min.
5. the preparation process of load flax oil nano emulsions as described in claim 1, which is characterized in that described in step (3)
The energy density of ultrasonication is 7200~10800J/mL.
6. the preparation process of load flax oil nano emulsions as described in claim 1, which is characterized in that described in step (3)
The condition of ultrasonication is that frequency is 20~30KHz, and power is 400~600W.
7. the preparation process of load flax oil nano emulsions as described in claim 1, which is characterized in that in step (3), super
During sonicated, using lasting or interval ultrasound mode, ultrasonic time is 10~25min.
8. the preparation process of load flax oil nano emulsions as described in claim 1, which is characterized in that it further include step (4),
Specifically: after nanoemulsions are freeze-dried or spray drying treatment of linseed oil is loaded described in step (3), obtains nanometer
Particle.
9. preparation process as described in any one of claims 1 to 7 is obtained to load flax oil nano emulsions.
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