CN102406721A - Oil-in-water type compound apple seed oil nano emulsion composition and preparation method thereof - Google Patents
Oil-in-water type compound apple seed oil nano emulsion composition and preparation method thereof Download PDFInfo
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- CN102406721A CN102406721A CN2011103767115A CN201110376711A CN102406721A CN 102406721 A CN102406721 A CN 102406721A CN 2011103767115 A CN2011103767115 A CN 2011103767115A CN 201110376711 A CN201110376711 A CN 201110376711A CN 102406721 A CN102406721 A CN 102406721A
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- eugenol
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Abstract
The invention discloses an oil-in-water type compound apple seed oil nano emulsion and a preparation method thereof. The composition comprises the following substances by mass percent:32.03-37.13% of surfactant, 0.01-5.23% of apple seed oil, 0.01-4.59% of eugenol, 0.01-6.55% of carvacrol and the balance of distilled water. The oil-in-water type compound apple seed oil nano emulsion composition, of which the appearance is yellow or faint yellow liquid and the liquid drop diameter ranges from 1nm to 100nm, has very good stability, wettability and percutaneous effect, and improves the bioavailability of apple seed oil, eugenol and carvacrol; and the medicament metabolism time of the composition in vivo is postponed.
Description
Technical field
The invention belongs to field of medicaments, relate to a kind of can anti-inflammation, sterilization antiseptical apple seed oil; The compound medicine novel form of eugenol and carvacrol; Be particularly related to a kind of oil-in-water type compound apple seed oil of clear, eugenol, and the nano emulsion composition of carvacrol and preparation method thereof.
Background technology
China is the high oil plant big producing countries of unsaturated fatty acid such as apple seed oil, and only the annual production of Shaanxi Fructus Mali pumilae seed is 10,000 tons, and resource is very abundant.The Fructus Mali pumilae seed contains multiple nutritional components, is a kind of ideal health food.Contained active component plant sterol in the Fructus Mali pumilae seed has anti-inflammation, and physiological functions such as immunomodulating are increasingly extensive in the application of field of medicaments.
Eugenol is colourless or pale yellow liquid, and intensive Flos Caryophylli fragrance is arranged, and is water insoluble, be mainly used in antibiotic, blood pressure lowering.Eugenol has very strong sterilizing power, can be used for dental caries as Bangesic, and has local antisepsis concurrently.
Carvacrol is a 2-hydroxyl cymene, has the colourless of thymol abnormal smells from the patient to be soluble in pure and mild ether to faint yellow stiff oily liquids, and is water-soluble hardly.Can volatilize with water vapour.The carvacrol bactericidal effect is good, can be used as sanitary disinfecting agent, anthelmintic, antiseptic.
But because water oil is immiscible, and traditional quintessence oil is simple extracting solution, and assimilation effect is poor, and bioavailability is low.
Summary of the invention
To problem that exists in the above-mentioned prior art and defective, the object of the present invention is to provide a kind of medicine stability high, bioavailability is high, and the oil-in-water type compound apple seed oil nano emulsion composition that dissolubility is high, slow-releasing is good.
The technical scheme that realizes the foregoing invention purpose is an oil-in-water type compound apple seed oil nano emulsion composition, and it is made up of the material of following mass percent:
Surfactant 32.030%～37.13%
Apple seed oil 0.01%～5.23%
Eugenol 0.01%～4.59%
Carvacrol 0.01%～6.55%
Surplus is a distilled water, and the mass percent summation of above-mentioned substance is 100%.
The present invention selects the nonionic surfactant of avirulence and good biocompatibility for use.Nonionic surfactant is more stable in solution, is not subject to the influence of strong electrolyte, inorganic salts, also is not subject to the influence of soda acid, and good with the compatibility of other surfactants, and haemolysis is less.Consider the easy formation property of nano-emulsion and the stability of the nano-emulsion for preparing, the present invention selects the liquid nonionic surfactant of HLB between 10～15 for use.Available surfactant has: any one of polyoxyethylene (40) castor oil hydrogenated (RH40), polyoxyethylene (40) Oleum Ricini (EL40), tween 80.
A further object of the invention provides the method for preparing of above-mentioned compound recipe apple seed oil nano emulsion composition, specifically may further comprise the steps:
1) it is subsequent use to take by weighing apple seed oil, eugenol, carvacrol, surfactant, distilled water;
2) apple seed oil, eugenol, carvacrol are mixed as oil phase;
3) surfactant is added in the oil phase stir, make its mix homogeneously and dropwise drip distilled water, until forming the oil-in-water type nano-emulsion.
The stability test of compound recipe apple seed oil nano emulsion composition of the present invention
1) ageing stability
Ageing stability is meant when nano-emulsion is preserved under room temperature nature change condition, and outward appearance prolongs and the degree that changes in time.The result shows that the compound nanometer emulsion compositions is transparent lastingly, does not find muddy or deposition, explains that ageing stability is good.This is an important indicator estimating nano-emulsion.
2) light stability test
Get an amount of compound recipe Nano medication liquid and blank Nano medication liquid and pack in the penicillin vial, be positioned over irradiation 10d under the daylight, in 1d, 3d, 5d, 10d sampling.The result shows that compound recipe Nano medication liquid still keeps clear, and color is yellow or colourless, no change.Blank nanometer medicinal liquid is clear still, is yellow or colourless, layering do not occur, wild effects such as muddiness.
) heat storage stability
Compound recipe oleum Cunninghamiae lanceolatae nano emulsion composition is placed test tube, and sealing places 37 ℃ of constant water bath box to store 14 days, this compound recipe nanometer medicinal liquid heat storage back appearance transparent, and no wild effect takes place.
4
) anti-freeze-stable property
With this compound recipe oleum Cunninghamiae lanceolatae nano emulsion composition in refrigerator-4 ℃ preserve a week after.Return to room temperature.If nano-emulsion becomes solids at-4 ℃, return to room temperature, return to transparently, and it is transparent to place all continued, thinks that then freezing-resistance is good.Through observing, this compound nanometer emulsion is stable to be thought well.
) CENTRIFUGAL ACCELERATING stability
This compound recipe oleum Cunninghamiae lanceolatae nano emulsion composition is placed test tube, and sealing under the rotating speed of 15000r/min centrifugal 20 minutes, does not have layering, still clear.
The purposes of compound recipe apple seed oil nano emulsion composition of the present invention
Compound recipe apple seed oil nano emulsion composition has tangible antibacterial and anti-inflammation functions, also immunity-regulating power.
Oil-in-water type compound oleum Cunninghamiae lanceolatae nano emulsion composition of the present invention compared with prior art has the following advantages:
1) thermodynamic stability is high, during preparation operation fairly simple, clear, does not precipitate not phase-splitting, bin stability improves;
2) be isotropic transparency liquid, through pressure sterilizing or centrifugally can not make it layering;
3) particle diameter is little, and between 1 ~ 100nm, transdermal effect is good, and penetrating power is strong, and porous advances skin performance drug effect and is easy to absorb.
4) had good sustained release effect can delay apple seed oil, eugenol, the regression time of the active component of carvacrol, thus improved above-mentioned quintessence oil bioavailability.
5) method technology is simple, is fit to large-scale production.
The practical implementation method
Test Example 1 compound recipe apple seed oil nano emulsion composition and folk prescription quintessence oil fungistatic effect contrast test
Inhibition zone is measured:
(1) adopt disk diffusion method, respectively 10% compound recipe apple seed oil nano emulsion composition, 10% apple seed oil folk prescription quintessence oil, 10% eugenol folk prescription quintessence oil, 10% carvacrol folk prescription quintessence oil supplied sample.
(2) under the aseptic condition, (d=6mm) immerse in the sample that has taken by weighing is behind the taking-up natural air drying will to justify filter paper; Be attached on the culture medium flat plate of smearing suitable bacterial concentration bacteria suspension 3 in every ware (d=9 cm), 3 repetitions of each test liquid; Divide and in 3 culture dishs, accomplish; Every ware central authorities compare with acetone, and plate places under the incubator thermophilic and cultivates, observed result.
(3) behind the 24h, be regarded as having fungistatic effect and measure the inhibition zone size the inhibition zone extract to occur.
Experimental result is as follows:
Compound nanometer emulsion and folk prescription quintessence oil inhibitory effect contrast (antibacterial circle diameter mm)
| Sample | Staphylococcus aureus | Escherichia coli | Bacillus subtilis |
| Compound recipe apple seed oil nano emulsion composition | 20.80 | 16.90 | 23.05 |
| 10% apple seed oil | 12.30 | 9.00 | 14.50 |
| 10% eugenol | 6.50 | 4.56 | 8.60 |
| 10% carvacrol | 18.9 | 15.94 | 16.87 |
| The ethanol contrast | 5.00 | 5.00 | 5.00 |
Can be known that by table prepared compound recipe apple seed oil nano emulsion composition, 10% apple seed oil folk prescription quintessence oil, 10% eugenol folk prescription quintessence oil, 10% carvacrol folk prescription quintessence oil are to escherichia coli and staphylococcus aureus, bacillus subtilis all has inhibitory action; Inhibitory effect is compared, and compound recipe apple seed oil nano emulsion composition is all big than folk prescription quintessence oil to the inhibition ability of three kinds of bacterium.
Minimum inhibitory concentration (MIC) is measured:
This experiment with the antibacterial mixed dissolution of variable concentrations in nutrient broth medium; Inoculated bacteria then; Through bacterial growth whether; Confirm to press down the least concentration that (resisting) microbial inoculum suppresses to be tried bacteria growing, i.e. minimal inhibitory concentration (MIC, the minimum inhibitory concentration).Experimental strain is selected staphylococcus aureus for use, escherichia coli and bacillus subtilis.Broth bouillon is by meat extract 1%, peptone 1%, sodium chloride 0.5%, distilled water 100ml configuration, the pH debugging for 7.4. behind strain pipe subcultivation, switching is 2 times in the meat soup pipe, as using strain, is 1 * 10 with the bacterial concentration dilution with 18h ~ 24h culture
8Individual/ml, use bacterial suspension as test.
(1) contains antibacterial culture medium configuration: compound recipe apple seed oil nano emulsion composition is become the test solution that receives of 0.1ug/ml ~ 10ug/ml variable concentrations with distilled water diluting, get each dilution factor and joined in the test tube that contains the double concentration nutrient broth of 1ml by test solution 1ml.
(2) get in the test tube that the 0.1ml bacterial suspension is inoculated in the nutrient broth that contains compound recipe apple seed oil nano emulsion composition, as the experimental group sample.
(3) in kind inoculated bacteria in the test tube of the nutrient broth that does not contain any medicine, as the negative control group sample.
(4) in kind inoculated bacteria in the test tube of the nutrient broth that contains blank nano-emulsion, as blank nano-emulsion check sample.
(5) in kind inoculated bacteria in the nutrient broth test tube that contains menthocamphorate, as the positive controls sample.
(6) medicament-carried nano breast sample, blank nano-emulsion sample, positive controls sample and negative control group sample are placed in 37 ℃ of incubators, cultivated observed result and record 48 hours.Not having pairing (resisting) bacteria suspension concentration that presses down of bacteria growing fully with each experimental group is the MIC that this sample correspondence is tried bacterium.
Experimental result is as shown in the table:
Compound recipe oleum Cunninghamiae lanceolatae nano-emulsion is to the minimal inhibitory concentration of three kinds of antibacterials
The result shows that compound recipe apple seed oil nano emulsion composition and positive controls compare, and effective percentage difference is extremely remarkable, and three kinds of antibacterials are had the obvious suppression effect.
Verify its superiority experiment
(1) with transmission electron microscope compound recipe apple seed oil nano emulsion composition of the present invention is carried out microscopic observation, can see that the nanometer emulsion droplet for spherical, is evenly distributed good dispersion, and big or small homogeneous.
(1) measure nano-emulsion of the present invention with Particle Size Analyzer, find that its particle size distribution is even, < particle diameter < 30nm accounts for 80%, particle diameter>30nm accounts for 16% to 10nm, and < 10nm accounts for 4% to particle diameter, and distribution is little, and particle diameter is less.
Explain that compound recipe apple seed oil nano emulsion composition particle diameter is less, bioavailability is high.
Embodiment 1
1) it is subsequent use to take by weighing 2.52% apple seed oil, 2.56% eugenol, 3.35% carvacrol, 37.13% surfactant, 54.47% distilled water;
2) apple seed oil, eugenol, carvacrol are mixed as oil phase;
3) surfactant is added in the oil phase stir, make its mix homogeneously and dropwise drip distilled water, until forming the oil-in-water type nano-emulsion.
Embodiment 2
Form by apple seed oil 0.01%, eugenol 4.59%, carvacrol 0.01%, EL-40 32.03%, distilled water 63.36%.
Embodiment 3
Form by apple seed oil 5.23%, eugenol 0.01%, carvacrol 3.21%, tween 80 33.00%, distilled water 58.55%.
Embodiment 4
Form by apple seed oil 3.82%, eugenol 3.82%, carvacrol 5.10%, tween 80 32.79%, distilled water 54.47%.
Embodiment 5
Form by apple seed oil 2.37%, eugenol 2.37%, carvacrol 3.16%, tween 80 37.00%, distilled water 55.10%.
Embodiment 6
Form by apple seed oil 3.66%, eugenol 3.66%, carvacrol 4.88%, RH-40 34.45%, distilled water 53.35%.
Embodiment 7
Form by apple seed oil 2.30%, eugenol 0.76%, carvacrol 3.83%, tween 80 36.64%, distilled water 56.47%.
Embodiment 8
Form by apple seed oil 3.83%, eugenol 1.27%, carvacrol 4.39%, EL-40 33.56%, distilled water 56.95%.
Embodiment 9
Form by apple seed oil 0.50%, eugenol 0.87%, carvacrol 4.37%, RH-40 33.56%, distilled water 60.07%.
Embodiment 10
Form by apple seed oil 5.23%, eugenol 1.30%, carvacrol 6.54%, tween 80 32.35%, distilled water 54.57%.
Embodiment 11
Form by apple seed oil 3.19%, eugenol 0.79%, carvacrol 3.99%, tween 80 33.12%, distilled water 58.91%.
Embodiment 12
Form by apple seed oil 4.96%, eugenol 1.24%, carvacrol 6.20%, RH-40 33.25%, distilled water 54.35%.
Claims (2)
1. compound recipe apple seed oil nano emulsion composition; It is characterized in that; Said composition is made up of the material of following mass percent: surfactant 32.030%～37.13%; Apple seed oil 0.01%～5.23%, eugenol 0.01%～4.59%, carvacrol 0.01%～6.55%, surplus are distilled water, and the mass percent summation of above-mentioned substance is 100%;
Described surfactant is a tween 80, any among RH-40, the EL-40.
2. the method for preparing of the described compound recipe apple seed oil of claim 1 nano emulsion composition is characterized in that, comprises the following steps:
1) it is subsequent use to take by weighing apple seed oil, eugenol, carvacrol, surfactant, distilled water;
2) apple seed oil, eugenol, carvacrol are mixed as oil phase;
3) surfactant is added in the oil phase stir, make its mix homogeneously and dropwise drip distilled water, until forming the oil-in-water type nano-emulsion.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107197860A (en) * | 2016-03-17 | 2017-09-26 | 新加坡国立大学 | Nano-emulsion containing carvacrol and preparation method thereof |
| CN113317431A (en) * | 2021-06-11 | 2021-08-31 | 扬州大学 | Oil-in-water carvacrol nanoemulsion and preparation method thereof |
| CN113796393A (en) * | 2020-06-17 | 2021-12-17 | 迈迪生物科技有限公司 | Environment-friendly essential oil emulsion with lasting slow release capacity and preparation method and application thereof |
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| CN1592578A (en) * | 2001-10-04 | 2005-03-09 | 以色列国家农业部富卡尼中心 | Microbiocidal formulation comprising essential oils or their derivatives |
| CN1931293A (en) * | 2006-09-21 | 2007-03-21 | 西北农林科技大学 | Oil-in-water type nanometer grassleaved sweetflag oil emulsion oral liquid and its prepn process |
| CN101214355A (en) * | 2007-12-29 | 2008-07-09 | 西北农林科技大学 | Compound eugenol nano emulsion composition and preparation thereof |
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2011
- 2011-11-24 CN CN2011103767115A patent/CN102406721A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1592578A (en) * | 2001-10-04 | 2005-03-09 | 以色列国家农业部富卡尼中心 | Microbiocidal formulation comprising essential oils or their derivatives |
| CN1931293A (en) * | 2006-09-21 | 2007-03-21 | 西北农林科技大学 | Oil-in-water type nanometer grassleaved sweetflag oil emulsion oral liquid and its prepn process |
| CN101214355A (en) * | 2007-12-29 | 2008-07-09 | 西北农林科技大学 | Compound eugenol nano emulsion composition and preparation thereof |
Non-Patent Citations (1)
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| 杨继红: "苹果籽油CO2超临界萃取及微胶囊化研究", 《中国优秀硕士学位论文全文数据库》, no. 5, 31 December 2007 (2007-12-31), pages 51 - 7 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107197860A (en) * | 2016-03-17 | 2017-09-26 | 新加坡国立大学 | Nano-emulsion containing carvacrol and preparation method thereof |
| CN107197860B (en) * | 2016-03-17 | 2021-12-07 | 新加坡国立大学 | Nanometer emulsion containing carvacrol and preparation method thereof |
| CN113796393A (en) * | 2020-06-17 | 2021-12-17 | 迈迪生物科技有限公司 | Environment-friendly essential oil emulsion with lasting slow release capacity and preparation method and application thereof |
| CN113317431A (en) * | 2021-06-11 | 2021-08-31 | 扬州大学 | Oil-in-water carvacrol nanoemulsion and preparation method thereof |
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Application publication date: 20120411 |