CN105168129A - Vitamin E nanoemulsion and preparation method thereof - Google Patents
Vitamin E nanoemulsion and preparation method thereof Download PDFInfo
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- CN105168129A CN105168129A CN201510453825.3A CN201510453825A CN105168129A CN 105168129 A CN105168129 A CN 105168129A CN 201510453825 A CN201510453825 A CN 201510453825A CN 105168129 A CN105168129 A CN 105168129A
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Abstract
The invention provides a vitamin E nanoemulsion and a preparation method thereof. The vitamin E nanoemulsion comprises vitamin E and dodecyl trimethylamine ammonium chloride of which the mass ratio is 1 to 2-7, dodecyl trimethylamine ammonium chloride, polyethylene glycol-400 and gummi tragacanthae of which the mass ratio is 1.5-4.5 to 0.5 to 0.5, as well as distilled water of which the mass is 1 to 5 times the total mass of the vitamin E and the dodecyl trimethylamine ammonium chloride. According to the invention, the process is simple, the conditions are mild, the preparation time is short, and equipment requirements are low. The prepared Vitamin E nanoemulsion is a clear and transparent liquid which is oil-in-water, excellent in water solubility and good in stability, the particle size distribution of the Vitamin E nanoemulsion ranges from 10 nm to 85 nm, the average grain diameter is 45nm, and the Vitamin E nanoemulsion conforms to essential characteristics of nanometer grade materials.
Description
Technical field
The invention belongs to feed additive field, particularly a kind of preparation method of vitamin E nano-emulsion.
Background technology
Vitamin E (VitaminE) is a kind of fatsoluble vitamin, and vitamin E has scavenging free radicals, enhancing human body immunity power, prevention reproductive system disease and improves the physiological function such as reproductive capacity and hatching of breeding eggs rate.Most of vitamin E product is all the esters derivative that chemical property is comparatively stable in the market, wherein common with Vitamin E acetate.Vitamin E series products is widely used in the industries such as food, cosmetic, pharmacy and livestock-raising, but due to vitamin E water insoluble, bioavailability is lower, significantly limit its application, applying particularly in livestock-raising.At present, vitamin E has been made into different types of products such as capsule, Emulsion, liposome, pre-mixing agent, suspensoid, wherein be most widely used with vitamin E suspensoid, suspensoid is because particle diameter is large, poor stability, bioavailability are low, and effect is not fine.And the preparation of vitamin Emulsion adopts the method for high pressure homogenizer to produce more, owing to being subject to the impact of high temperature in process of production, the content of vitamin E reduces a lot, causes very large loss.
Nano-emulsion be spontaneously to be formed by water, emulsifying agent, co-emulsifier and wet goods, particle diameter is at the Thermodynamically stable of 1 ~ 100nm, isotropic transparent or semitransparent dispersed system.Nano-emulsion has that viscosity is low, bioavailability is high, slow release and targeting, belong to thermodynamically metastable fixed system, and preparation method is simple, has become one of focus of feed additive and novel pharmaceutical formulation research.
Because current vitamin E exists above-mentioned a series of shortcoming deficiency, bring very large difficulty to livestock and poultry cultivation and clinical practice, therefore researching and developing above-mentioned shortcoming deficiency that employing new technique overcomes vitamin E is one of this field scientific research technical staff new problem anxious to be resolved.
Summary of the invention
The object of the invention is to overcome above-mentioned weak point, the preparation method of the vitamin E nano-emulsion that a kind of technique is simple, good water solubility, steady quality, bioavailability are high is provided.
For achieving the above object, the technical solution adopted in the present invention is as follows: a kind of vitamin E nano-emulsion, comprising mass ratio is 1:(2-7) vitamin E and dodecyl trimethylamine ammonium chloride, mass ratio is the dodecyl trimethylamine ammonium chloride of (1.5-4.5): 0.5:0.5, PEG-4000 and tragakanta, and mass ratio be vitamin E and dodecyl trimethylamine ammonium chloride gross mass and 1-5 distilled water doubly.
A preparation method for vitamin E nano-emulsion, carry out as follows:
(1) in container, add vitamin E and dodecyl trimethylamine ammonium chloride in mass ratio, stir;
(2) in (1), add PEG-4000 and tragakanta in mass ratio, stir;
(3) in (2), add distilled water in mass ratio, stir, obtain the vitamin E nano-emulsion of clear.
The invention has the beneficial effects as follows:
Its technique is simple, and mild condition, preparation time is short, and equipment requirements is low.Vitamin E nano-emulsion water solublity prepared by this method is good, good stability, and its particle size distribution range is between 10nm ~ 85nm, and mean diameter is 45nm, meets the basic feature of nanometer materials.
The selection of raw material of the present invention and the restriction of consumption, be the crucial part that the present invention prepares nano-emulsion, the interphase interaction of raw material, coordinates preparation method of the present invention, prepares the vitamin E nano-emulsion of water solublity, good stability.
Detailed description of the invention
Below in conjunction with preferred embodiment, to according to detailed description of the invention provided by the invention, details are as follows:
Embodiment 1
A preparation method for vitamin E nano-emulsion, carry out as follows:
(1) 1:2 adds vitamin E and dodecyl trimethylamine ammonium chloride in container in mass ratio, stirs;
(2) be that 1.5:0.5:0.5 adds PEG-4000 and tragakanta in (1) according to the mass ratio of dodecyl trimethylamine ammonium chloride, PEG-4000 and tragakanta, stir;
(3) according to mass ratio be vitamin E and dodecyl trimethylamine ammonium chloride gross mass and 1 times in (2), add distilled water, stir, obtain the vitamin E nano-emulsion of clear.
Embodiment 2
A preparation method for vitamin E nano-emulsion, carry out as follows:
(1) 1:4.5 adds vitamin E and dodecyl trimethylamine ammonium chloride in container in mass ratio, stirs;
(2) be that 3:0.5:0.5 adds PEG-4000 and tragakanta in (1) according to the mass ratio of dodecyl trimethylamine ammonium chloride, PEG-4000 and tragakanta, stir;
(3) according to mass ratio be vitamin E and dodecyl trimethylamine ammonium chloride gross mass and 3 times in (2), add distilled water, stir, obtain the vitamin E nano-emulsion of clear.
Embodiment 3
A preparation method for vitamin E nano-emulsion, carry out as follows:
(1) 1:7 adds vitamin E and dodecyl trimethylamine ammonium chloride in container in mass ratio, stirs;
(2) be that 4.5:0.5:0.5 adds PEG-4000 and tragakanta in (1) according to the mass ratio of dodecyl trimethylamine ammonium chloride, PEG-4000 and tragakanta, stir;
(3) according to mass ratio be vitamin E and dodecyl trimethylamine ammonium chloride gross mass and 5 times in (2), add distilled water, stir, obtain the vitamin E nano-emulsion of clear.
Embodiment 4
A preparation method for vitamin E nano-emulsion, carry out as follows:
(1) 1:4 adds vitamin E and dodecyl trimethylamine ammonium chloride in container in mass ratio, stirs;
(2) be that 2.5:0.5:0.5 adds PEG-4000 and tragakanta in (1) according to the mass ratio of dodecyl trimethylamine ammonium chloride, PEG-4000 and tragakanta, stir;
(3) according to mass ratio be vitamin E and dodecyl trimethylamine ammonium chloride gross mass and 2.5 times in (2), add distilled water, stir, obtain the vitamin E nano-emulsion of clear.
Embodiment 5
A preparation method for vitamin E nano-emulsion, carry out as follows:
(1) 1:5.5 adds vitamin E and dodecyl trimethylamine ammonium chloride in container in mass ratio, stirs;
(2) be that 4:0.5:0.5 adds PEG-4000 and tragakanta in (1) according to the mass ratio of dodecyl trimethylamine ammonium chloride, PEG-4000 and tragakanta, stir;
(3) according to mass ratio be vitamin E and dodecyl trimethylamine ammonium chloride gross mass and 4 times in (2), add distilled water, stir, obtain the vitamin E nano-emulsion of clear.
The particle size determination of vitamin E nano-emulsion:
The present invention adopts laser scattering technology, the particle diameter of DLS-700 type laser light scattering instrument to nanometer vitamin E using Japanese great Zhong electronics corporation to produce measures, test temperature 25.7 DEG C during measurement, optical maser wavelength 632.8nm, testing result is that particle size distribution range is between 10nm ~ 85nm, mean diameter is 45nm, meets the basic feature of nanometer materials.
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Particle diameter (nm) | 46.5 | 45 | 43.5 | 42.6 | 47.4 |
Below the water solublity of vitamin E nano-emulsion prepared by the present invention and stability are investigated.
1, the soluble test of vitamin E nano-emulsion:
Vitamin E nano-emulsion prepared by embodiment 1-5 method can be soluble in water with arbitrary proportion rapidly, and solution clear, free from admixture, illustrate that vitamin E nano-emulsion water solublity is good.
2, the stability test of vitamin E nano-emulsion:
According to Pharmacopoeia of the People's Republic of China version appended claims in 2000, vitamin E nano-emulsion prepared by embodiment 1-5 method centrifugal 15 minutes with 4000r/min, all do not observe lamination, prove that the stability of vitamin E nano-emulsion prepared by embodiment 1-5 method meets the requirements.
2.1, physical stability is investigated
2.1.1 centrefuge experiment
Adopt centrifugal steadiness parameter method, get 50 milliliters of centrifuge tubes and be respectively charged into vitamin E nano-emulsion to be measured 30 milliliters, centrifugal 10 minutes, 20 minutes and 30 minutes are distinguished with 2000r/min, the diluent measuring rovitamin E nano-emulsion respectively descends the absorbance of liquid layer at wavelength 532nm place afterwards with being separated, and calculates centrifugal steadiness parameter Ke.The results are shown in Table 1.
Ke＝(A
0-A)/A
0×100％
A
0for the diluent of rovitamin E nano-emulsion is at the absorbance of a certain wavelength.
A is the absorbance at Same Wavelength after rovitamin E nano-emulsion centrifuge tube lower floor after centrifugal dilutes through same times.
The stability parameter of the vitamin E nano-emulsion under table 1 centrifugal test different time
| Time | 0 minute | 10 minutes | 20 minutes | 30 minutes |
| Embodiment 1 Ke | 0.012 | 0.012 | 0.102 | 0.103 |
| Embodiment 2 Ke | 0.012 | 0.012 | 0.101 | 0.102 |
| Embodiment 3 Ke | 0.012 | 0.012 | 0.102 | 0.104 |
| Embodiment 4 Ke | 0.012 | 0.013 | 0.104 | 0.104 |
| Embodiment 5 Ke | 0.012 | 0.012 | 0.102 | 0.104 |
Test shows, the centrifugal steadiness parameter Ke value of centrifugal test on vitamin E nano-emulsion does not almost affect.
2.1.2 jolting test
Respectively get 10 milliliters of vitamin E nano-emulsion, fill nitrogen, be sealed in 25 milliliters of test tubes, 100rpm jolting in 25 DEG C of water bath with thermostatic control agitators, respectively in 12h, 24h, 48h, 72h sampling, measure the centrifugal steadiness parameter Ke of vitamin E nano-emulsion under each sample time.The results are shown in Table 2.
The stability parameter of vitamin E nano-emulsion under the table 2 different jolting time
| Time | 0 hour | 12 hours | 24 hours | 48 hours | 72 hours |
| Embodiment 1 Ke | 0.012 | 0.012 | 0.074 | 0.105 | 0.109 |
| Embodiment 2 Ke | 0.012 | 0.012 | 0.072 | 0.103 | 0.109 |
| Embodiment 3 Ke | 0.012 | 0.013 | 0.074 | 0.102 | 0.110 |
| Embodiment 4 Ke | 0.011 | 0.014 | 0.076 | 0.106 | 0.108 |
| Embodiment 5 Ke | 0.011 | 0.013 | 0.075 | 0.104 | 0.110 |
Test shows, the centrifugal steadiness parameter Ke value impact of continuous jolting on vitamin E nano-emulsion is little.
2.1.3 hot test
Vitamin E nano-emulsion is filled nitrogen, sealing, place 10 days respectively under the conditions of 40 DEG C, 60 DEG C, 70 DEG C, investigated the size and distribution of vitamin E nano-emulsion respectively at 0 day, 5 days, 10 days.Result of the test is in table 3.
Table 3 different temperatures is on the impact of vitamin E nano-emulsion particle diameter
Test shows, under different temperatures to vitamin E nano-emulsion particle diameter without significant change, but long-time storage should avoid high temperature.
2.1.4 accelerated test
Vitamin E nano-emulsion is placed 6 months under the condition of temperature 40 DEG C, investigates the particle size distribution of the vitamin E nano-emulsion of 1 month, 2 months, 3 months, 6 months.Result of the test is in table 4.
Table 4 accelerated test is on the impact of vitamin E nano-emulsion particle diameter
| Time/moon | 0 | 1 | 2 | 3 | 6 |
| Embodiment 1 particle diameter/nm | 46.5±12 | 47.8±13 | 48.9±18 | 52.1±10 | 53.4±12 |
| Embodiment 2 particle diameters/nm | 45±12 | 46.1±12 | 46.9±13 | 47.2±10 | 49.4±14 |
| Embodiment 3 particle diameters/nm | 43.5±11 | 44.8±11 | 45.9±18 | 48.2±10 | 51.3±11 |
| Embodiment 4 particle diameters/nm | 42.9±12 | 43.8±14 | 44.5±11 | 47.3±14 | 54.1±15 |
| Embodiment 5 particle diameters/nm | 47.4±10 | 48.4±14 | 49.7±12 | 52.4±16 | 54.5±15 |
Test shows, under accelerated test condition, the particle diameter of vitamin E nano-emulsion is without significant change.
2.2 chemical stability tests
2.2.1 influence factor's test
Vitamin E nano-emulsion is filled nitrogen, sealing, place 10 days respectively under the conditions of 40 DEG C, 60 DEG C, 70 DEG C, investigated the changes of contents of vitamin E nano-emulsion respectively at 0 day, 5 days, 10 days.Result of the test is in table 5.
The changes of contents of vitamin E nano-emulsion under table 5 condition of different temperatures
Result of the test shows, vitamin E nano-emulsion is placed under these experimental conditions, the content of vitamin E within the storage life without significant change.
2.2.2 accelerated test
Vitamin E nano-emulsion is placed 6 months under the condition of temperature 40 DEG C, investigates the changes of contents of the vitamin E nano-emulsion of 1 month, 2 months, 3 months, 6 months.Result of the test is in table 6.
Table 6 accelerated test is on the impact of vitamin E nano milk content
| Time/moon | 0 | 1 | 2 | 3 | 6 |
| Embodiment 1 content % | 99.5 | 99.2 | 98.4 | 98.0 | 97.5 |
| Embodiment 2 content % | 99.8 | 99.4 | 98.8 | 98.4 | 97.9 |
| Embodiment 3 content % | 99.3 | 99.2 | 98.9 | 98.5 | 97.8 |
| Embodiment 4 content % | 98.3 | 98.3 | 98.2 | 98.1 | 97.3 |
| Embodiment 5 content % | 99.5 | 99.4 | 99.2 | 98.7 | 97.1 |
Test shows, under accelerated test condition, the content of vitamin E nano-emulsion is without significant change.
Contrast test:
Comparative example 1:
In order to obtain good vitamin E nano-emulsion concentration, We conducted the nano-emulsion test of vitamin E, choose from anion surfactant, zwitterionic surfactant, non-ionic surface active agent, cationic surfactant by representational surfactant respectively, carried out nano-emulsion contrast test.Experimental result is in table 7.
Several surfactant of table 7 is on the impact of vitamin E nano-emulsion
The nano-emulsion that cationic surfactant dodecyl trimethylamine ammonium chloride is formed is better, and in addition, it also has certain antibacterial action and the tolerance effect to light, heat, acid, alkali etc., therefore selects dodecyl trimethylamine ammonium chloride as surfactant.
Comparative example 2:
In order to obtain better vitamin E nano-emulsion, We conducted the screening of cosurfactant, with to the stability influence of vitamin E nano-emulsion and cosurfactant consumption for index carries out screening test.Result of the test is in table 8.
The different cosurfactant of table 8 is tested the impact of vitamin E nano-emulsion
| Cosurfactant title | Glycerol | Ethanol | PEG-400 | PEG-600 | Tragcanth |
| Nano-emulsion stability | Stable | Stable | Stable | Unstable | Stable |
| Cosurfactant consumption (g) | 20 | 18 | 5 | 25 | 5 |
As can be seen here, when adopting cosurfactant PEG-400 and tragcanth, the nano-emulsion of formation is more stable, and the consumption of cosurfactant is also minimum, so both save the consumption of cosurfactant, turn avoid environmental pollution and the pessimal stimulation to poultry body.
Comparative example 3:
In order to obtain better vitamin E nano-emulsion, We conducted two kinds of cosurfactant compound proportions and the impact of nano-emulsion is tested.Result of the test is in table 9.
Table 9 two kinds of cosurfactant compound proportions are tested the impact of nano-emulsion
| Ratio (PEG/ tragakanta) | 2:1 | 4:3 | 1:1 | 3:5 | 1:2 |
| Mean diameter (nm) | 112 | 56 | 45 | 67 | 87 |
| Content of vitamin E (%) | 89.2 | 90.1 | 99.8 | 91.4 | 87.9 |
As can be seen here, when the ratio of PEG/ tragakanta is 1:1, the nano-emulsion particle diameter of formation is minimum, and content of vitamin E is the highest.
In a word, above-mentioned series of experiments shows, the physical and chemical index of vitamin E nano-emulsion, without significant change, has good stability.
Above-mentioned detailed description of the preparation method of vitamin E nano-emulsion being carried out with reference to embodiment; illustrative instead of determinate; several embodiments can be listed according to institute's limited range; therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.
Claims (2)
1. a vitamin E nano-emulsion, it is characterized in that: comprising mass ratio is 1:(2-7) vitamin E and dodecyl trimethylamine ammonium chloride, mass ratio is the dodecyl trimethylamine ammonium chloride of (1.5-4.5): 0.5:0.5, PEG-4000 and tragakanta, and mass ratio be vitamin E and dodecyl trimethylamine ammonium chloride gross mass and 1-5 distilled water doubly.
2. a preparation method for vitamin E nano-emulsion according to claim 1, is characterized in that carrying out as follows:
(1) in container, add vitamin E and dodecyl trimethylamine ammonium chloride in mass ratio, stir;
(2) in (1), add PEG-4000 and tragakanta in mass ratio, stir;
(3) in (2), add distilled water in mass ratio, stir, obtain the vitamin E nano-emulsion of clear.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101057829A (en) * | 2006-04-21 | 2007-10-24 | 上海医药工业研究院 | Supersaturated cationic self-emulsified drug delivery system and its preparation method |
| CN101703468A (en) * | 2009-11-30 | 2010-05-12 | 浙江大学 | Nano-emulsion of vitamin E oil and preparation method thereof |
| CN103520103A (en) * | 2013-10-14 | 2014-01-22 | 陕西科技大学 | Vitamin E nano-emulsion and preparation method thereof |
| CN104207145A (en) * | 2014-09-18 | 2014-12-17 | 苏州经贸职业技术学院 | Vitamin E nano-microemulsion and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057829A (en) * | 2006-04-21 | 2007-10-24 | 上海医药工业研究院 | Supersaturated cationic self-emulsified drug delivery system and its preparation method |
| CN101703468A (en) * | 2009-11-30 | 2010-05-12 | 浙江大学 | Nano-emulsion of vitamin E oil and preparation method thereof |
| CN103520103A (en) * | 2013-10-14 | 2014-01-22 | 陕西科技大学 | Vitamin E nano-emulsion and preparation method thereof |
| CN104207145A (en) * | 2014-09-18 | 2014-12-17 | 苏州经贸职业技术学院 | Vitamin E nano-microemulsion and preparation method thereof |
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Denomination of invention: Vitamin E nano-emulsion and preparation method thereof Effective date of registration: 20200426 Granted publication date: 20180223 Pledgee: Qilu bank Limited by Share Ltd. Ji'nan Changqing branch Pledgor: SHANDONG SOOCOM ANIMAL REMEDY Co.,Ltd. Registration number: Y2020980001803 |
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