CN110623846A - Method for preparing oil-in-water lecithin nanoemulsion and nanoemulsion obtained by same - Google Patents
Method for preparing oil-in-water lecithin nanoemulsion and nanoemulsion obtained by same Download PDFInfo
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
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Abstract
The present invention provides a method for preparing an oil-in-water lecithin nanoemulsion, wherein the method comprises the steps of: 1) dispersing lecithin in an oil phase, adding a part of a water phase, and stirring to form a gel state to form a first lecithin multiphase gel; 2) adding another part of water phase into the first lecithin multiphase gel to carry out first-stage high-pressure homogenization to obtain a second lecithin multiphase gel; and 3) adding the second lecithin multiphase gel into water for secondary high-pressure homogenization to obtain the oil-in-water lecithin nanoemulsion. The invention also provides the oil-in-water lecithin nanoemulsion obtained by the method.
Description
Technical Field
The invention provides a method for preparing oil-in-water lecithin nanoemulsion and the oil-in-water lecithin nanoemulsion obtained by the method.
Background
In 1844 Gohley, French, discovered lecithin from egg yolk and was named Lecithos (lecithin) in Greek. Lecithin is a mixture of animal and plant tissues and yolk, and is a yellow brown greasy substance, and its components include phosphoric acid, choline, fatty acid, glycerol, glycolipid, triglyceride and phospholipid.
Lecithin is an important component of cell membranes and has extremely high biocompatibility. Lecithin is broadly defined as a variety of phospholipid products, including Phosphatidylcholine (PC), Phosphatidylethanolamine (PE), Phosphatidic Acid (PA), Phosphatidylinositol (PI), etc., and in the narrow sense, lecithin refers to phosphatidylcholine. The higher the purity of PC, the smaller the odor and the stronger the emulsifying property. The lecithin has a tail with a double-hydrophobic structure, can be directly dispersed in water to form vesicles which are in an ordered phospholipid bilayer structure, so that the lecithin meets the condition of an emulsifier in the surfactant and can serve as the emulsifier to a certain extent.
However, lecithin is a low-polarity oleaginous substance, insoluble in water, wherein high-purity lecithin (phosphatidylcholine > 90%) is insoluble even in general vegetable oils and fats. Therefore, the application of high-purity lecithin in cosmetics is difficult.
In the prior art, lecithin is mainly used for preparing liposome, microemulsion and nanoemulsion, wherein the preparation process of the liposome is complicated, alcohol is generally required to be added as a solvent, and the preparation method is not friendly to cosmetic compositions and preparation processes. The existing microemulsion and nanoemulsion technologies need to be compounded with other surfactants, and high-purity lecithin cannot be independently used for preparing stable emulsion.
Therefore, there is an urgent need to develop a method for preparing an oil-in-water lecithin nanoemulsion and an oil-in-water lecithin nanoemulsion obtained thereby.
Disclosure of Invention
The inventor surprisingly finds that the nano-emulsion of the lecithin can be realized by a multi-stage high-pressure homogenization technology and a relay emulsification method. The method for preparing the oil-in-water lecithin nanoemulsion can be used for industrial production of cosmetics.
Accordingly, in one aspect, the present invention provides a method for preparing an oil-in-water lecithin nanoemulsion, wherein the method comprises the steps of:
1) dispersing lecithin in an oil phase, adding a part of a water phase, and stirring to form a gel state to form a first lecithin multiphase gel;
2) adding another part of water phase into the first lecithin multiphase gel to carry out first-stage high-pressure homogenization to obtain a second lecithin multiphase gel; and
3) and adding the second lecithin multiphase gel into water for secondary high-pressure homogenization to obtain the oil-in-water lecithin nanoemulsion.
According to a preferred embodiment of the present invention, the aqueous phase is selected from at least one of water, glycerol and glycol.
According to a preferred embodiment of the present invention, the diol may be selected from at least one of 1, 3-propanediol, 1, 2-propanediol, 1, 3-butanediol, 1, 2-pentanediol, and 1, 2-hexanediol.
According to a preferred embodiment of the invention, said portion of the aqueous phase is a glycol; the other part of the aqueous phase is selected from glycerol and water.
According to another preferred embodiment of the invention, the oil phase is selected from at least one of squalane, sunflower oil, olive oil, jojoba oil and cetearyl alcohol.
According to a preferred embodiment of the invention, when the oil phase is selected from squalane and the portion of the aqueous phase is selected from 1, 3-propanediol and the other portion of the aqueous phase is selected from glycerol and water, the process comprises the following steps:
1) dispersing lecithin in squalane, adding 1, 3-propylene glycol, and stirring to form gel, so as to obtain three-phase gel of lecithin, squalane and 1, 3-propylene glycol;
2) adding glycerol and water into the lecithin, squalane and 1, 3-propylene glycol three-phase gel to carry out first-stage high-pressure homogenization to obtain lecithin, squalane, glycerol and 1, 3-propylene glycol four-phase gel; and
3) and adding the lecithin, squalane, glycerol and 1, 3-propylene glycol four-phase gel into water for secondary high-pressure homogenization to obtain the oil-in-water lecithin nanoemulsion.
According to a preferred embodiment of the present invention, the weight content ratio of lecithin to squalane to 1, 3-propanediol three-phase gel in the lecithin, squalane and 1, 3-propanediol three-phase gel of the above step 1) is 1-5:1-20:1-5, preferably 1-1.5:1-10: 1-5.
The invention relates to a multistage high-pressure homogenization technology, which is a technology for performing multiple high-pressure homogenization to carry out lecithin molecule nanocrystallization in the emulsification process. The inventor surprisingly found that oil-in-water lecithin nanoemulsion with average particle size of about 100nm can be obtained by performing multiple high-pressure homogenization to make lecithin molecules into nano-particles. If the first-stage high-pressure homogenization is skipped, the particle size of the prepared emulsion droplets cannot reach 100nm even if the cycle number of the second-stage high-pressure homogenization is increased by 2 times.
The intermediate emulsification method of the present invention is a method of forming an intermediate composition during the preparation of a lecithin emulsion, and then adding an aqueous phase to emulsify the intermediate composition, i.e., the first lecithin multiphase gel and the second lecithin multiphase gel of the present invention. According to a preferred embodiment of the invention, the first and second lecithin multiphase gels are a lecithin, squalane and 1, 3-propanediol three-phase gel and a lecithin, squalane, glycerol and 1, 3-propanediol four-phase gel, respectively.
A second aspect of the present invention provides an oil-in-water lecithin nanoemulsion obtained according to the method, wherein the average particle size of the oil-in-water lecithin nanoemulsion is around 100 nm.
According to a preferred embodiment of the present invention, the oil-in-water lecithin nanoemulsion comprises: 65-95 wt% of an aqueous phase, 1-30 wt% of an oil phase and 1-5 wt% of lecithin.
According to another preferred embodiment of the present invention, the oil-in-water lecithin nanoemulsion comprises: 75-90 wt% of an aqueous phase, 5-25 wt% of an oil phase and 1-3 wt% of lecithin.
According to a preferred embodiment of the present invention, the aqueous phase is selected from at least one of water, glycerol and glycol.
According to a preferred embodiment of the present invention, the diol may be selected from at least one of 1, 3-propanediol, 1, 2-propanediol, 1, 3-butanediol, 1, 2-pentanediol, and 1, 2-hexanediol.
According to another preferred embodiment of the invention, the oil phase is selected from at least one of squalane, sunflower oil, olive oil and jojoba oil.
According to a particularly preferred embodiment of the present invention, the oil-in-water lecithin nanoemulsion comprises: 50-70 wt% of water, 10-30 wt% of glycerol, 1-30 wt% of squalane, 1-5 wt% of 1, 3-propanediol and 1-5 wt% of lecithin.
More preferably, the oil-in-water lecithin nanoemulsion comprises: 50-70 wt% of water, 10-30 wt% of glycerol, 1-30 wt% of squalane, 1-5 wt% of 1, 3-propanediol and 1-1.5 wt% of lecithin.
According to a most preferred embodiment of the present invention, the oil-in-water lecithin nanoemulsion consists of 50 to 70% by weight of water, 10 to 30% by weight of glycerol, 1 to 30% by weight of squalane, 1 to 5% by weight of 1, 3-propanediol and 1 to 5% by weight of lecithin.
More preferably, the oil-in-water lecithin nanoemulsion consists of 50 to 70 wt% of water, 10 to 30 wt% of glycerin, 1 to 30 wt% of squalane, 1 to 5 wt% of 1, 3-propanediol, and 1 to 1.5 wt% of lecithin.
The method for preparing the oil-in-water lecithin nanoemulsion and the oil-in-water lecithin nanoemulsion obtained by the method have the advantages that:
1. the method for preparing the oil-in-water lecithin nanoemulsion realizes the nanocrystallization of lecithin emulsion by a multi-stage high-pressure homogenization technology and a relay emulsification method, and can obtain the blue light nanoemulsion with uniform particle size and stable system;
2. the oil-in-water lecithin nanoemulsion has the average particle size of about 100 nanometers, so that the oil-in-water lecithin nanoemulsion has good stability and can be stored for a long time, and therefore, the oil-in-water lecithin nanoemulsion can be used for industrial production of cosmetics;
3. the invention activates the emulsifying property of lecithin through a relay emulsifying method, and can maintain the stability of the oil-in-water lecithin nanoemulsion under the condition of not compounding other emulsifiers, thereby greatly expanding the application of the lecithin in cosmetics.
Drawings
FIG. 1 is a nano-emulsion of oil-in-water lecithin prepared in example 1.
FIG. 2 is a graph showing the particle size distribution of the oil-in-water lecithin nanoemulsion prepared in example 1 by two-stage high pressure homogenization as measured by a beckman LSI3320 dynamic light scattering particle size distribution instrument.
FIG. 3 is a particle size distribution as measured by beckman LSI3320 dynamic light scattering particle size distribution instrument of the oil-in-water lecithin nanoemulsion prepared in comparative example 2 using only 2 times of the second stage high pressure homogenization cycle.
Detailed Description
Example 1: preparation of the oil-in-water lecithin nanoemulsion of the invention
| Serial number | Name of Chinese | Content (g) |
| 1 | Water (W) | 68 |
| 2 | Glycerol | 20 |
| 3 | Cetostearyl alcohol | 10 |
| 4 | 1,2 pentanediol | 1 |
| 5 | Lecithin | 1 |
The preparation method comprises the following steps: adding 1g of lecithin into 10g of cetearyl alcohol and 1,2 g of pentanediol, stirring, dissolving and dispersing, adding 20g of glycerol, homogenizing to obtain multiphase gel, carrying out first-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company, adding 69g of water, and carrying out second-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company to obtain the oil-in-water lecithin nanoemulsion.
Example 2: preparation of the oil-in-water lecithin nanoemulsion of the invention
| Serial number | Name of Chinese | Content (g) |
| 1 | Water (W) | 63 |
| 2 | Glycerol | 30 |
| 3 | Squalane | 5 |
| 4 | 1, 3-propanediol | 1 |
| 5 | Lecithin | 1 |
The preparation method comprises the following steps: adding 1g of lecithin into 5g of squalane and 1g of 1, 3-propylene glycol, stirring, dissolving and dispersing, adding 30g of glycerol, homogenizing to obtain multiphase gel, carrying out first-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company, adding 63g of water, and carrying out second-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company to obtain the oil-in-water lecithin nanoemulsion.
Example 3: preparation of the oil-in-water lecithin nanoemulsion of the invention
| Serial number | Name of Chinese | Content (g) |
| 1 | Water (W) | 30 |
| 2 | Glycerol | 30 |
| 3 | Jojoba oil | 30 |
| 4 | 1, 3-butanediol | 5 |
| 5 | Lecithin | 5 |
The preparation method comprises the following steps: adding 5g of lecithin into 30g of jojoba oil and 5g of 1, 3-propylene glycol, stirring, dissolving, dispersing, adding 30g of glycerol, homogenizing to obtain multiphase gel, performing first-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company, adding 30g of water, and performing second-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company to obtain the oil-in-water lecithin nanoemulsion.
Example 4: preparation of the oil-in-water lecithin nanoemulsion of the invention
| Serial number | Name of Chinese | Content (g) |
| 1 | Water (W) | 57 |
| 2 | Glycerol | 30 |
| 3 | Squalane | 10 |
| 4 | 1, 2-hexanediol | 1.5 |
| 5 | Lecithin | 1.5 |
The preparation method comprises the following steps: adding 1.5g lecithin into 10g squalane and 1.5g 1, 3-propylene glycol, stirring, dissolving, dispersing, adding 30g glycerol, homogenizing to obtain multiphase gel, performing first-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company, adding 57g water, and performing second-stage high-pressure homogenization by an SPX-1000 high-pressure homogenizer of APV company to obtain the oil-in-water lecithin nanoemulsion.
Comparative example 1: preparation of oil-in-water nanoemulsion by using sucrose laurate as emulsifier
| Serial number | Name of Chinese | Content (g) |
| 1 | Water (W) | 58 |
| 2 | Glycerol | 30 |
| 3 | Squalane | 10 |
| 4 | 1, 3-propanediol | 1 |
| 5 | Sucrose laurate | 1 |
The preparation method comprises the following steps: adding sucrose laurate 1g into water 58g and propylene glycol 1, 3-and glycerol 30g, stirring to dissolve, heating to 60-65 deg.C, adding squalane 10g, homogenizing, and homogenizing under high pressure with SPX-1000 high pressure homogenizer of APV company to obtain oil-in-water nanoemulsion.
Comparative example 2: oil-in-water lecithin nanoemulsion prepared by adopting 2 times of second-stage high-pressure homogenization circulation
| Serial number | Name of Chinese | Content (g) |
| 1 | Water (W) | 68 |
| 2 | Glycerol | 20 |
| 3 | Cetostearyl alcohol | 10 |
| 4 | 1,2 pentanediol | 1 |
| 5 | Lecithin | 1 |
The preparation method comprises the following steps: adding 1g of lecithin into 10g of cetearyl alcohol and 1,2 g of pentanediol, stirring, dissolving and dispersing, adding 20g of glycerol, homogenizing to obtain multiphase gel, adding 69g of water, and performing secondary high-pressure homogenization circulation by 2 times through an SPX-1000 high-pressure homogenizer of APV company to obtain the oil-in-water lecithin nanoemulsion.
Experimental example 1
The lecithin nanoemulsion prepared in examples 1-4 of the present invention was placed in a biological incubator at 5 deg.C, 40 deg.C, circulating (-5-40 deg.C, cycle 24h) and room temperature, and observed every other week, and the results are shown in the following table.
The above results show that the lecithin nanoemulsion prepared in the embodiments 1-4 of the present invention can be kept stable for three months at 5 ℃, 40 ℃, circulation (-5-40 ℃, cycle 24h) biological incubator and room temperature, and thus meets the stability requirement. Therefore, the lecithin nanoemulsion of the invention can maintain the stability of the oil-in-water lecithin nanoemulsion without being compounded with other emulsifiers.
Experimental example 2: evaluation of emulsifying Capacity of lecithin nanoemulsion prepared in examples 1 to 4 of the present invention
The emulsifying capacity of each lecithin nanoemulsion described above was first evaluated by a conventional centrifugation test at 2000rpm/min for 30min at 25 ℃. To further evaluate the relative emulsifying ability of each of the above lecithin nanoemulsions, a high temperature centrifugation experiment was performed at 2000rpm/min at 40 ℃ until reaching the centrifugal breakdown point thereof for each of the lecithin nanoemulsions without delamination after the conventional centrifugation experiment.
Additionally, comparative example 1, made with sucrose laurate, was used as a control.
The emulsifying ability comparison results are lecithin nanoemulsion of example 2 > lecithin nanoemulsion of example 4 > lecithin nanoemulsion of example 3 > lecithin nanoemulsion of example 1 ≈ lecithin nanoemulsion of comparative example 1. In general, the emulsifying ability of the oil-in-water lecithin nanoemulsion of the present invention was substantially equivalent to that of comparative example 1 containing an emulsifier, and reached the requirement of the minimum emulsifying ability that the emulsifier must have as a cosmetic composition, and thus it was possible to use in the industrial production of emulsifier-free cosmetic compositions without compounding other emulsifiers.
Experimental example 3: the particle size distribution measured by a beckman LSI3320 dynamic light scattering particle size distribution instrument of the oil-in-water lecithin nanoemulsion prepared by adopting two-stage high-pressure homogenization in the embodiment 1 of the invention and the particle size distribution measured by a beckman LSI3320 dynamic light scattering particle size distribution instrument of the oil-in-water lecithin nanoemulsion prepared by adopting 2 times of the second-stage high-pressure homogenization circulation in the comparative example 2.
First, FIGS. 2 and 3 show the particle size distributions measured by a beckman LSI3320 dynamic light scattering particle size distribution instrument of the oil-in-water lecithin nanoemulsion prepared by the two-stage high-pressure homogenization of example 1 according to the present invention and the oil-in-water lecithin nanoemulsion prepared by comparative example 2 using only the second-stage high-pressure homogenization cycle 2 times, respectively. Those skilled in the art will appreciate that particle size distribution testing is performed by diluting the sample 20-50 times with deionized water and adding to a beckman LSI3320 dynamic light scattering particle size distribution meter.
As can be seen from fig. 2 and 3, the oil-in-water lecithin nanoemulsion prepared by the two-stage high-pressure homogenization of example 1 according to the present invention shows a single peak with a narrow distribution and an average particle size of about 100nm, while the oil-in-water lecithin nanoemulsion prepared by the second-stage high-pressure homogenization cycle of comparative example 2 only shows a single peak with a wide distribution and a poor uniformity with an average particle size of about 0.5 μm. Therefore, the oil-in-water lecithin nanoemulsion prepared by adopting the second-stage high-pressure homogenization is obviously superior to the sample prepared by only adopting the second-stage high-pressure homogenization in particle size and uniformity.
Therefore, the method for preparing the oil-in-water lecithin nanoemulsion realizes the nanocrystallization of the lecithin emulsion through a multi-stage high-pressure homogenization technology, and can obtain the blue light nanoemulsion with uniform particle size and stable system.
Claims (16)
1. A method of preparing an oil-in-water lecithin nanoemulsion, wherein the method comprises the steps of:
1) dispersing lecithin in an oil phase, adding a part of a water phase, and stirring to form a gel state to form a first lecithin multiphase gel;
2) adding another part of water phase into the first lecithin multiphase gel to carry out first-stage high-pressure homogenization to obtain a second lecithin multiphase gel;
3) and adding the second lecithin multiphase gel into water for secondary high-pressure homogenization to obtain the oil-in-water lecithin nanoemulsion.
2. The method of preparing an oil-in-water lecithin nanoemulsion according to claim 1, wherein the aqueous phase is selected from at least one of water, glycerol, and glycol.
3. The method for preparing an oil-in-water lecithin nanoemulsion according to claim 2, wherein the diol is selected from at least one of 1, 3-propanediol, 1, 2-propanediol, 1, 3-butanediol, 1, 2-pentanediol, and 1, 2-hexanediol.
4. The method of preparing an oil-in-water lecithin nanoemulsion according to claim 1, wherein the portion of the aqueous phase is a glycol.
5. The method for preparing an oil-in-water lecithin nanoemulsion according to claim 1, wherein the other part of the aqueous phase is glycerol and water.
6. The method of preparing an oil-in-water lecithin nanoemulsion according to claim 1, wherein the oil phase is selected from at least one of squalane, sunflower oil, olive oil, jojoba oil and cetearyl alcohol.
7. A method of preparing an oil-in-water lecithin nanoemulsion, wherein the method comprises the steps of:
1) dispersing lecithin in squalane, adding 1, 3-propylene glycol, and stirring to form gel, so as to obtain three-phase gel of lecithin, squalane and 1, 3-propylene glycol;
2) adding glycerol and water into the lecithin, squalane and 1, 3-propylene glycol three-phase gel to carry out first-stage high-pressure homogenization to obtain lecithin, squalane, glycerol and 1, 3-propylene glycol four-phase gel; and
3) and adding the lecithin, squalane, glycerol and 1, 3-propylene glycol four-phase gel into water for secondary high-pressure homogenization to obtain the oil-in-water lecithin nanoemulsion.
8. The method for preparing an oil-in-water lecithin nanoemulsion according to claim 7, wherein the weight content ratio of lecithin to squalane to 1, 3-propanediol three-phase gel in the lecithin, squalane and 1, 3-propanediol three-phase gel of step 1) is 1-5:1-20: 1-5.
9. An oil-in-water lecithin nanoemulsion obtained according to the method of any one of claims 1-8, wherein the average particle size of the oil-in-water lecithin nanoemulsion is around 100 nm.
10. The oil-in-water lecithin nanoemulsion of claim 9, wherein the lecithin nanoemulsion comprises: 65-95 wt% of an aqueous phase, 1-30 wt% of an oil phase and 1-5 wt% of lecithin.
11. The oil-in-water lecithin nanoemulsion of claim 9, wherein the lecithin nanoemulsion comprises: 75-90 wt% of an aqueous phase, 5-25 wt% of an oil phase and 1-3 wt% of lecithin.
12. The oil-in-water lecithin nanoemulsion of claim 10 or 11, wherein the aqueous phase is selected from at least one of water, glycerol and glycol.
13. The oil-in-water lecithin nanoemulsion of claim 12, wherein the diol is selected from at least one of 1, 3-propanediol, 1, 2-propanediol, 1, 3-butanediol, 1, 2-pentanediol, and 1, 2-hexanediol.
14. The oil-in-water lecithin nanoemulsion of claim 10 or 11, wherein the oil phase is selected from at least one of squalane, sunflower oil, olive oil, jojoba oil and cetearyl alcohol.
15. The oil-in-water lecithin nanoemulsion according to claim 10 or 11, wherein the lecithin nanoemulsion comprises: 50-70 wt% of water, 10-30 wt% of glycerol, 1-30 wt% of squalane, 1-5 wt% of 1, 3-propanediol and 1-5 wt% of lecithin.
16. The oil-in-water lecithin nanoemulsion according to claim 10 or 11, wherein the lecithin nanoemulsion consists of 50-70% by weight of water, 10-30% by weight of glycerol, 1-30% by weight of squalane, 1-5% by weight of 1, 3-propanediol and 1-5% by weight of lecithin.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111671662A (en) * | 2020-07-01 | 2020-09-18 | 江苏瑞蓓丽生物科技有限公司 | Preparation method of nanoemulsion for improving vitreous factor bioavailability |
| CN115590783A (en) * | 2022-09-16 | 2023-01-13 | 上海百雀羚生物科技有限公司（Cn） | Method for preparing oil-in-water type micro-emulsion by reverse emulsification and application of oil-in-water type micro-emulsion in cosmetics |
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- 2019-10-17 CN CN201910986258.6A patent/CN110623846A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111671662A (en) * | 2020-07-01 | 2020-09-18 | 江苏瑞蓓丽生物科技有限公司 | Preparation method of nanoemulsion for improving vitreous factor bioavailability |
| CN111671662B (en) * | 2020-07-01 | 2022-03-29 | 江苏瑞蓓丽生物科技有限公司 | Preparation method of nanoemulsion for improving vitreous factor bioavailability |
| CN115590783A (en) * | 2022-09-16 | 2023-01-13 | 上海百雀羚生物科技有限公司（Cn） | Method for preparing oil-in-water type micro-emulsion by reverse emulsification and application of oil-in-water type micro-emulsion in cosmetics |
| CN115590783B (en) * | 2022-09-16 | 2024-03-22 | 上海百雀羚生物科技有限公司 | Method for preparing oil-in-water type micro emulsion by reverse emulsion and application of oil-in-water type micro emulsion in cosmetics |
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