CN112168737A - Nano emulsion and preparation method thereof - Google Patents
Nano emulsion and preparation method thereof Download PDFInfo
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- 239000007908 nanoemulsion Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 27
- 150000003904 phospholipids Chemical class 0.000 claims abstract description 26
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims abstract description 20
- 229920002385 Sodium hyaluronate Polymers 0.000 claims abstract description 20
- 229940010747 sodium hyaluronate Drugs 0.000 claims abstract description 20
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims abstract description 20
- 239000000787 lecithin Substances 0.000 claims abstract description 14
- 235000010445 lecithin Nutrition 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 229940067606 lecithin Drugs 0.000 claims abstract description 13
- 239000012141 concentrate Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 5
- 239000012071 phase Substances 0.000 claims description 73
- 239000003921 oil Substances 0.000 claims description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 27
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- 235000019437 butane-1,3-diol Nutrition 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- WCVRQHFDJLLWFE-UHFFFAOYSA-N pentane-1,2-diol Chemical compound CCCC(O)CO WCVRQHFDJLLWFE-UHFFFAOYSA-N 0.000 claims description 6
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 5
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 5
- 239000000194 fatty acid Substances 0.000 claims description 5
- 229930195729 fatty acid Natural products 0.000 claims description 5
- 150000004665 fatty acids Chemical class 0.000 claims description 5
- 150000002191 fatty alcohols Chemical class 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 claims description 5
- 229920005862 polyol Polymers 0.000 claims description 5
- 150000003077 polyols Chemical class 0.000 claims description 5
- 239000001993 wax Substances 0.000 claims description 5
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 claims description 4
- 229940015975 1,2-hexanediol Drugs 0.000 claims description 4
- 229940035437 1,3-propanediol Drugs 0.000 claims description 4
- FHKSXSQHXQEMOK-UHFFFAOYSA-N hexane-1,2-diol Chemical compound CCCCC(O)CO FHKSXSQHXQEMOK-UHFFFAOYSA-N 0.000 claims description 4
- 229920000166 polytrimethylene carbonate Polymers 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 239000008346 aqueous phase Substances 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 10
- 239000003995 emulsifying agent Substances 0.000 abstract description 9
- 238000003756 stirring Methods 0.000 description 11
- 235000011187 glycerol Nutrition 0.000 description 8
- 239000000839 emulsion Substances 0.000 description 7
- 239000002537 cosmetic Substances 0.000 description 6
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 6
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 description 2
- BANXPJUEBPWEOT-UHFFFAOYSA-N 2-methyl-Pentadecane Chemical compound CCCCCCCCCCCCCC(C)C BANXPJUEBPWEOT-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- ATGQXSBKTQANOH-UWVGARPKSA-N N-oleoylphytosphingosine Chemical compound CCCCCCCCCCCCCC[C@@H](O)[C@@H](O)[C@H](CO)NC(=O)CCCCCCC\C=C/CCCCCCCC ATGQXSBKTQANOH-UWVGARPKSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 description 2
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 2
- 229960001631 carbomer Drugs 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 description 2
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 description 2
- 229960002216 methylparaben Drugs 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- -1 polydimethylsiloxane Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229940099259 vaseline Drugs 0.000 description 2
- 239000000230 xanthan gum Substances 0.000 description 2
- 229920001285 xanthan gum Polymers 0.000 description 2
- 229940082509 xanthan gum Drugs 0.000 description 2
- 235000010493 xanthan gum Nutrition 0.000 description 2
- 229940043268 2,2,4,4,6,8,8-heptamethylnonane Drugs 0.000 description 1
- 241001530056 Athelia rolfsii Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- KUVMKLCGXIYSNH-UHFFFAOYSA-N isopentadecane Natural products CCCCCCCCCCCCC(C)C KUVMKLCGXIYSNH-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229940042880 natural phospholipid Drugs 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 230000008591 skin barrier function Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/55—Phosphorus compounds
- A61K8/553—Phospholipids, e.g. lecithin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/068—Microemulsions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Molecular Biology (AREA)
- Biophysics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Emergency Medicine (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a nano-emulsion and a preparation method thereof, wherein the nano-emulsion contains phospholipid, polyalcohol, an oil phase, sodium hyaluronate and a water phase; the preparation method comprises the following steps: A. uniformly dispersing phospholipid in polyalcohol and water, heating to 40-80 deg.C, and preparing to obtain water phase; B. heating the oil phase to 40-80 ℃, and uniformly mixing to obtain an oil phase; C. slowly adding the oil phase prepared in the step B into the water phase prepared in the step A, and emulsifying the oil phase with the mean value to obtain a prepared emulsified body; D. c, adding a sodium hyaluronate aqueous solution into the emulsified body prepared in the step C, and uniformly dispersing to obtain a prepared nano emulsion concentrated body; E. d, adding a water phase into the nano emulsion concentrate prepared in the step D to obtain the prepared nano emulsion; the invention improves the existing low-energy consumption method for preparing the nano emulsion, uses lecithin of natural source as an emulsifier, widens the oil selection range and prepares the stable nano emulsion.
Description
Technical Field
The invention relates to the field of cosmetics, in particular to a nano emulsion and a preparation method thereof.
Background
In the cosmetic field, emulsions are generally composed of an aqueous phase, an oil phase and an emulsifier, and have a particle size of generally 1 to 50 μm, and are classified into oil-in-water (O/W) type, water-in-oil (W/O) type and multiple emulsion type. The emulsifying system belongs to a thermodynamically unstable system, and unstable phenomena such as layering, aggregation, flocculation and the like are easy to occur. Compared with the traditional emulsion, the nano emulsion has smaller particle size which is usually between 20 and 500 nm, belongs to a thermodynamically unstable system, but has better kinetic stability, so that the phenomena of layering and aggregation are not easy to occur. In addition, the nanoemulsion can improve the water solubility and transdermal absorption capacity of the oil-soluble active substance, improve the activity of antioxidant and the like, and can be applied to formulations such as water aqua, cream, spray, gel, aerosol and the like, so that the nanoemulsion becomes a carrying and shaping system with great application prospects in the fields of cosmetics and the like.
Currently, the common methods for preparing nano-emulsion are divided into two categories: one is a High-energy method, and the other is a Low-energy method. The high energy consumption method requires special equipment such as a high pressure homogenizer, a micro-jet machine or an ultrasonic jet homogenizer to provide high enough energy to produce the nano-emulsion with fine particle size; since the high energy process requires special emulsification equipment and very little energy (about 0.1%) is used for the emulsification process, most is lost in the form of heat energy. Compared with the prior art, the low-energy consumption method utilizing the chemical energy can greatly reduce the cost and the investment, but only certain grease and emulsifier can form stable nano emulsion by utilizing the low-energy consumption method, which greatly limits the application of the low-energy consumption method. Furthermore, the low energy method requires a higher content of chemical emulsifiers, which poses certain irritation and safety risks.
Phospholipid is an amphiphilic substance of natural origin, has certain emulsifying property and is also a main component of cell membranes. Therefore, the phospholipid is used as the emulsifier, has good affinity and safety to the skin when being applied to cosmetics, and also has the effects of repairing skin barriers and moistening the skin. The nano emulsion prepared by using phospholipid is also often used as a carrier to improve the transdermal permeability of active substances. Natural phospholipids are composed of a mixture of several phospholipids, which are broadly referred to as lecithins and phosphatidylcholine is narrowly referred to as lecithin. Since lecithin is very easily oxidized, the saturation of acyl groups can be increased by hydrogenation, and hydrogenated lecithin with good stability can be obtained.
Although lecithin is frequently used as an excellent emulsifier in cosmetics, in the existing nano-emulsion preparation technology, when lecithin is used as an emulsifier, a stable nano-emulsion cannot be prepared by using a conventional low-energy consumption method, while a high-energy consumption method requires special equipment and has a low energy utilization rate.
Disclosure of Invention
In order to solve the problems, the nano-emulsion preparation method provided by the invention uses natural lecithin as an emulsifier, and an improved low-energy-consumption method is used for preparing nano-emulsion, so that the energy utilization rate is improved, the selection range of grease is widened, and the safety and permeability of nano-emulsion are improved.
A method for preparing a nano emulsion is characterized by comprising the following steps:
A. uniformly dispersing phospholipid in polyalcohol and water, and heating to 40-80 deg.C to obtain water phase;
B. heating the oil phase to 40-80 ℃, and uniformly mixing to obtain the prepared oil phase;
C. slowly adding the oil phase prepared in the step B into the water phase prepared in the step A, and emulsifying the oil phase with the average value, wherein the homogenizing speed is 1000-;
D. c, adding a sodium hyaluronate aqueous solution into the emulsified body prepared in the step C, and uniformly dispersing to obtain a prepared nano emulsion concentrated body;
E. d, adding a water phase into the nano emulsion concentrate prepared in the step D to obtain the prepared nano emulsion;
wherein, the following components are prepared according to weight percentage before preparation:
in the step A, the content of phospholipid is 0.1-2%, the content of polyalcohol is 1-20%, the content of water is 0.1-10%,
in the step B, the oil phase content is 1-60%,
in the step D, the content of the sodium hyaluronate aqueous solution is 0.5-10 percent,
in the step E, the water phase content is 10-90%;
wherein, the phospholipid in the step A is any one of lecithin or hydrogenated lecithin, and the content of phosphatidylcholine is more than or equal to 60 percent; the polyhydric alcohol in the step A is any one or the combination of any two or more of glycerol, 1, 3-butanediol, 1, 3-propanediol, 1, 2-pentanediol, 1, 2-hexanediol, dipropylene glycol and PEG-8; the water in the step A is deionized water;
the oil phase in the step B is selected from any one or any combination of grease, wax, hydrocarbon, fatty acid, fatty alcohol, synthetic ester, silicone oil and oil solubility activity;
in the step D, the concentration of the sodium hyaluronate aqueous solution is 0.1-5%;
in step E, the water phase can be selected from deionized water and any other water-soluble components.
The phospholipid nanoemulsion with stable sodium hyaluronate prepared by the steps contains phospholipid, polyol, an oil phase, a sodium hyaluronate aqueous solution and a water phase; wherein the phospholipid content is 0.1-2%, the polyalcohol content is 1-20%, the oil phase content is 1-60%, the sodium hyaluronate content is 0.01-0.5%, and the water phase content is 10-90%;
the phospholipid is selected from any one of lecithin or hydrogenated lecithin, and the content of phosphatidylcholine is more than or equal to 60%;
the polyhydric alcohol is any one or the combination of any two or more of glycerol, 1, 3-butanediol, 1, 3-propanediol, 1, 2-pentanediol, 1, 2-hexanediol, dipropylene glycol and PEG-8;
the oil phase is selected from any one or any combination of oil, wax, hydrocarbon, fatty acid, fatty alcohol, synthetic ester, silicone oil and oil solubility activity;
and the particle size of the phospholipid nano emulsion with stable sodium hyaluronate prepared by the steps is 50-200 nm.
The invention has the positive effects of improving the existing low-energy consumption method for preparing the nano emulsion, taking the lecithin from natural sources as the emulsifier, preparing the nano emulsion by utilizing the improved low-energy consumption method, improving the energy utilization rate, widening the selection range of grease and improving the safety and the permeability of the nano emulsion.
The nano emulsion prepared by the invention has high stability, can be applied to dosage forms such as water aqua, cream, spray, gel, aerosol and the like, and becomes a carrying and shaping system with great application prospect in the fields of cosmetics and the like.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example 1:
in order to prepare the phospholipid nano-emulsion with stable sodium hyaluronate, the raw materials are prepared according to the following formula by weight percent:
phase A: 2% of water, 3% of 1, 2-pentanediol, 3% of 1, 3-butanediol and 0.3% of lecithin
Phase B: 3 percent of vaseline, 2 percent of polydimethylsiloxane, 0.5 percent of stearyl alcohol and 0.05 percent of ceramide III
And C phase: 0.05% of sodium hyaluronate and 5% of water
Phase D: 5% of glycerin, 0.2% of xanthan gum, 0.1% of methyl hydroxybenzoate, 0.05% of EDTA-2Na and 73.75% of water
The preparation method comprises the following steps:
heating phase A to 60 deg.C, and dispersing for 20 min;
heating phase B to 80 deg.C, and stirring;
adding phase B into phase A under stirring, and homogenizing at 3000rpm for 5 min;
adding the dispersed phase C into the phase AB, and uniformly mixing to obtain a nano emulsion concentrate;
mixing the D phase uniformly, cooling to room temperature, adding into the nano emulsion concentrate, and stirring uniformly.
To better demonstrate the technical result of the present invention, the following comparative example 1 is provided as a comparison with example 1:
comparative example 1: process for preparing conventional emulsions
Phase A: 3 percent of 1, 2-pentanediol, 3 percent of 1, 3-butanediol, 0.05 percent of sodium hyaluronate, 5 percent of glycerol, 0.2 percent of xanthan gum, 0.1 percent of methyl hydroxybenzoate, 0.05 percent of EDTA-2Na and 80.75 percent of water
Phase B: 3 percent of vaseline, 4 percent of polydimethylsiloxane, 0.5 percent of stearyl alcohol, 0.05 percent of ceramide III and 0.3 percent of lecithin
The preparation method of comparative example 1 is a commonly used emulsion preparation method: heating phase A and phase B to 80 deg.C respectively, adding phase B into phase A under stirring, homogenizing at 3000rpm for 5min, stirring, and cooling to room temperature.
The phospholipid emulsion prepared by a common emulsion preparation method has the particle size of 2-10 mu m, and is layered after standing for 24 hours; the phospholipid nanoemulsion prepared by the method has the particle size of 50-200nm and good stability after standing for 24 hours.
Example 2:
in order to prepare the phospholipid nano-emulsion with stable sodium hyaluronate, the raw materials are prepared according to the following formula by weight percent:
phase A: 6% of water, 85% of PEG, 4% of dipropylene glycol and 1.2% of hydrogenated lecithin
Phase B: 2% of glycerol triethyl hexanoate, 4% of cyclopenta dimethyl silicone polymer and 3% of isohexadecane
And C phase: 0.08 percent of sodium hyaluronate and 10 percent of water
Phase D: 6 percent of glycerin, 1 percent of trehalose, 0.2 percent of sclerotium rolfsii gum, 0.15 percent of carbomer, 0.1 percent of methylparaben, 0.05 percent of EDTA-2Na, 0.07 percent of aminomethyl propanol and 73.75 percent of water
The preparation method comprises the following steps:
1) heating phase A to 40 deg.C, and dispersing for 20 min;
2) heating phase B to 40 deg.C, and stirring;
3) adding phase B into phase A under stirring, and homogenizing at 8000rpm for 10 min;
4) adding the dispersed phase C into the phase AB, and uniformly mixing to obtain a nano emulsion concentrate;
5) mixing the D phase uniformly, cooling to room temperature, adding into the nano emulsion concentrate, and stirring uniformly.
The phospholipid nanoemulsion prepared by the method has the particle size of 50-200nm, is good in stability after standing for 24 hours at normal temperature, and does not delaminate after being centrifuged at 2000rpm for 30 min.
Example 3
Phase A: 0.1% of water, 1.3-propanediol, 0.1% of hydrogenated lecithin
Phase B: glycerol triethyl hexanoate 1%
And C phase: 0.01 percent of sodium hyaluronate and 10 percent of water
Phase D: 6 percent of glycerin, 1 percent of trehalose, 0.2 percent of carbomer, 0.1 percent of methylparaben, 0.05 percent of EDTA-2Na, 0.1 percent of aminomethyl propanol and 80.34 percent of water
The preparation method comprises the following steps:
1) heating phase A to 40 deg.C, and dispersing for 20 min;
2) heating phase B to 40 deg.C, and stirring;
3) adding phase B into phase A under stirring, and homogenizing at 20000rpm for 2 min;
4) adding the dispersed phase C into the phase AB, and uniformly mixing to obtain a nano emulsion concentrate;
5) mixing the D phase uniformly, cooling to room temperature, adding into the nano emulsion concentrate, and stirring uniformly.
The phospholipid nanoemulsion prepared by the embodiment has the particle size of 50-200nm, is good in stability after standing for 24 hours at normal temperature, and does not delaminate after being centrifuged at 2000rpm for 30 min.
In the above embodiments, the water phase according to the technical scheme of the present invention may adopt deionized water and any other water-soluble components, such as a humectant, a thickener, a preservative, etc.;
the oil phase in the technical scheme of the invention can adopt any one or any combination of oil, wax, hydrocarbon, fatty acid, fatty alcohol, synthetic ester, silicone oil and oil solubility activity;
the homogenizer adopted by the technical scheme of the invention can be a common homogenizer in the market, such as an IKA disperser, a PRIMIX high-shear emulsification disperser and the like.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make several improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims (15)
1. A nanoemulsion, characterized in that it contains a phospholipid.
2. The nanoemulsion of claim 1, further comprising a polyol, an oil phase, sodium hyaluronate, and an aqueous phase.
3. The nanoemulsion of claim 2, wherein the phospholipid content is 0.1-2%, the polyol content is 1-20%, the oil phase content is 1-60%, the sodium hyaluronate content is 0.01-0.5%, and the water phase content is 10-90%.
4. The nano-emulsion according to claim 3, wherein the phospholipid is selected from any one of lecithin and hydrogenated lecithin, and the content of phosphatidylcholine is not less than 60%.
5. The nano-emulsion according to claim 3, wherein the polyol is any one or a combination of any two or more of glycerol, 1, 3-butanediol, 1, 3-propanediol, 1, 2-pentanediol, 1, 2-hexanediol, dipropylene glycol, and PEG-8.
6. The nano-emulsion according to claim 3, wherein the oil phase is selected from any one of oils, waxes, hydrocarbons, fatty acids, fatty alcohols, synthetic esters, silicones, and oil-soluble activities, or any combination thereof.
7. A nanoemulsion as claimed in claim 3, characterised in that the aqueous phase is selected from deionised water and any other water-soluble components.
8. The nanoemulsion of claim 1, wherein the nanoemulsion ranges from 50 nm to 200nm in particle size.
9. A method for preparing a nano emulsion is characterized by comprising the following steps:
A. uniformly dispersing phospholipid in polyalcohol and water, and heating to 40-80 deg.C to obtain water phase;
B. heating the oil phase to 40-80 ℃, and uniformly mixing to obtain the prepared oil phase;
C. slowly adding the oil phase prepared in the step B into the water phase prepared in the step A, and emulsifying the oil phase with the average value, wherein the homogenizing speed is 1000-;
D. c, adding a sodium hyaluronate aqueous solution into the emulsified body prepared in the step C, and uniformly dispersing to obtain a prepared nano emulsion concentrated body;
E. and D, adding a water phase into the nano emulsion concentrate prepared in the step D to obtain the prepared nano emulsion.
10. The method of claim 9, wherein the nano-emulsion comprises the following components in percentage by weight:
in the step A, the content of phospholipid is 0.1-2%, the content of polyalcohol is 1-20%, and the content of water is 0.1-10%, wherein the water is deionized water;
in the step B, the oil phase content is 1-60%;
in the step D, the content of the sodium hyaluronate aqueous solution is 0.5-10%,
in the step E, the content of the water phase is 10-90%.
11. The method for preparing nano-emulsion according to claim 10, wherein the phospholipid in step A is selected from any one of lecithin and hydrogenated lecithin, and the content of phosphatidylcholine is not less than 60%.
12. The method of claim 11, wherein the polyol used in step a is selected from the group consisting of glycerol, 1, 3-butanediol, 1, 3-propanediol, 1, 2-pentanediol, 1, 2-hexanediol, dipropylene glycol, and PEG-8.
13. The method of claim 10, wherein the oil phase in step B is selected from any one of oils, waxes, hydrocarbons, fatty acids, fatty alcohols, synthetic esters, silicone oils, and oil-soluble activities, or any combination thereof.
14. The method of claim 10, wherein the concentration of the aqueous solution of sodium hyaluronate in step D is 0.1-5%.
15. The method of claim 10, wherein the water phase in step E is selected from deionized water and any other water-soluble components.
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