CN103393580A - Preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion - Google Patents
Preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion Download PDFInfo
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- CN103393580A CN103393580A CN2013103435960A CN201310343596A CN103393580A CN 103393580 A CN103393580 A CN 103393580A CN 2013103435960 A CN2013103435960 A CN 2013103435960A CN 201310343596 A CN201310343596 A CN 201310343596A CN 103393580 A CN103393580 A CN 103393580A
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- terminalia arjuna
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- tree bark
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Abstract
The invention relates to a preparation method for a Terminalia arjuna bark extract lipid nanoparticle emulsion. The preparation method is characterized by comprising the following steps: A, dissolving dry Terminalia arjuna bark extract powder in 1,2-pentanediol in proportion so as to obtain an alcoholic solution of a Terminalia arjuna bark extract; B, mixing the alcoholic solution with an emulsifier and glycerol monostearate, heating an obtained mixture to a temperature of 75 to 85 DEG C and carrying out stirring at a rotating speed of 650 r/min for 10 min; C, mixing the oil phase of a liquid obtained in step B with distilled water according to a ratio of 0.41-1.78: 1, heating to a temperature of 75 to 85 DEG C and carrying out stirring at a rotating speed of 650 r/min; and D, carrying out cyclic homogenization by using a high pressure homogenizer 8 to 15 times at a temperature of 75 to 85 DEG C and a pressure of 70 to 150 MPa and cooling to room temperature so as to obtain the Terminalia arjuna bark extract lipid nanoparticle emulsion. The Terminalia arjuna bark extract lipid nanoparticle emulsion prepared in the invention has the advantages of good stability, high bioavailability, substantial moisture retention and crease resistance effects when added in a formula for a cosmetic and convenience in cold formulation and addition of the emulsion into the cosmetic.
Description
Technical field
The present invention relates to the liposome technology field, particularly a kind of preparation method of Terminalia arjuna tree bark extract lipid nanoparticle emulsion.
Background technology
(the INCI title: the active component TERMINALIA ARJUNA) is mainly multiple olive alkanes triterpenoid to Terminalia arjuna tree bark extract, and wherein the most important thing is arjunolic acid (Arjunolic acid).Commercial Terminalia arjuna tree bark extract has been arranged at present, the arjunolic acid (Arjunolic acid) that wherein contains 80% purity, it is pentacyclic triterpenoid, and other 20% is mainly some tannins and Flavonoid substances, and the manufacturer is U.S. SABINSA company.Research finds that Terminalia arjuna tree bark extract has stronger antiinflammatory and antidotal effect, by strengthening the skin blood microcirculation, increase skin elasticity and dermis density, help to recover the natural sebum levels of skin after climacteric and can strengthen the skin barrier performance, make skin become more smooth, be applied in the cosmetic formulations application and show obvious moisturizing and crease-resistant effect.Terminalia arjuna tree bark extract is pure soluble substance, and it is less stable in cosmetic formulations, and bioavailability is low, easy oxidized variable color.In prior art, due to this specific character of Terminalia arjuna tree bark extract, cause its being greatly limited property of scope in application.Terminalia arjuna is set to bark extract and be prepared into the lipid nanoparticle emulsion, add in cosmetic formulations, its stability, range of application, bioavailability are improved.
Summary of the invention
The technical problem to be solved in the present invention is that a kind of preparation method of lipid nanoparticle emulsion of energy load Terminalia arjuna tree bark extract is provided; The lipid nanoparticle emulsion of Terminalia arjuna tree bark extract prepared by the inventive method can significantly improve stability and the bioavailability thereof of active matter, make Terminalia arjuna tree bark extract be not easy oxidized, the product efficacy conservation rate is high, facilitates cold joining to join in cosmetic formulations.
For solving the problems of the technologies described above, the present invention by the following technical solutions: the preparation method of a kind of Terminalia arjuna tree bark extract lipid nanoparticle emulsion is characterized in that comprising the following steps:
A: for the ratio of 0.5-1.0:1.0, Terminalia arjuna is set to bark extract dry powder in mass ratio and be dissolved in 1, the 2-pentanediol dissolves, and obtains Terminalia arjuna tree bark extract alcoholic solution;
B: be 0.15-0.80: 0.20-0.33 in mass ratio: 1 ratio, taking steps A gained Terminalia arjuna tree bark extract alcoholic solution, emulsifying agent and stearic acid monoglycerides mixes, mixed liquor is heated to 75-85 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirred 10 minutes, obtain the liquid oil phase of homogeneous; Described emulsifying agent is the mixture of PLURONICS F87, poloxamer188 and Natrulon H-10 myristinate, and in mixture, three's mass ratio is 0.10-0.75:0.10-0.75:1;
C: be in mass ratio 0.41-1.78: 1 ratio takes step B gained liquid oil phase and distilled water, mixes post-heating to 75-85 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirs, and obtains premixed solution;
D: step C gained premixed solution, under 75-85 ℃ of temperature conditions, 70-150MPa pressures cycle homogenizing 8-15 times, is cooled to room temperature by high pressure homogenizer, obtains Terminalia arjuna tree bark extract lipid nanoparticle emulsion.
The Terminalia arjuna tree bark extract lipid nanoparticle emulsion for preparing by the inventive method, comprise mass percent and be 1.0-8.0% Terminalia arjuna tree bark extract.
By Terminalia arjuna prepared by the inventive method, set bark extract lipid nanoparticle emulsion, under room temperature, viscosity, less than 1000cps, is easy to topple over, and can coldly join and join in cosmetic formulations, in moisturizing and crease-resistant effect cosmetics, as active additive, use easily; Terminalia arjuna tree bark extract lipid nanoparticle emulsion prepared by the inventive method is that in per minute 10000 centrifuges that turn, centrifugal 30min is not stratified at rotating speed; Under 45 ℃ of environment, preserve invariant color in three months, not stratified.Under room temperature, kept 3 years, invariant color, not stratified.
The nanoparticle particle diameter that the prepared Terminalia arjuna of the present invention is set in bark extract lipid nanoparticle emulsion can be controlled in the 65-150nm scope, have particle diameter little, be easy to the infiltration, stability and bioavailability thereof are improved, and facilitate the cold advantage that joins in cosmetic formulations of joining.
The test result of below testing for effect of the present invention:
1, keratodermatitis hydration rate test: sample adopts cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%), the cosmetics that directly add 5.0% Terminalia arjuna tree bark extract and the blank group cosmetics that add 10% bark extract of the Terminalia arjuna tree by embodiment tri-preparations lipid nanoparticle emulsion.
This method of testing is carried out according to the method that provides as Publication about Document: " foundation of cosmetic industry evaluation methodology ", Beijing daily use chemicals, the 4th phase in 2006,20-23 page, Zhao Hua, Dong Yinmao, He Congfen, Lan Sheyi, Wang Changtao.
The mensuration of keratodermatitis moisture: its operation principle is take capacitor as instrument probe, it due to water, is the material of dielectric constant maximum on skin, when skin moisture content changes, the capacitance of skin also changes, so can be by measuring skin capacitance, analyzing skin surface moisture content.Instrument commonly used is Corneometer CM825.By measurement, use the variation of product front and back keratodermatitis capacitance to weigh the variation of water content of stratum corneum, thereby estimate the moisture-keeping efficacy of cosmetics, this kind method is carried out quantification to the moisture of keratodermatitis, can react delicately the variation of skin moisture content, and favorable reproducibility is one of present moisture-keeping cosmetics effect evaluation method commonly used.
Experimental technique: bend the square Experimental Area that side marks 3 * 3cm2 size at candidate left and right forearm, using the test zone of left arm as moisturizer, the corresponding symmetrical region of right arm is blank, then with Corneometer CM825 tester, detect the moisture at each test position, repeat respectively 5 times, draw meansigma methods.With formula (1) calculated hydration rate.
Hydration rate=(test value-blank value)/blank value (1)
Experimental result sees the following form.Table A
Annotate: the blank group of A, the content that B directly adds Terminalia arjuna tree bark extract is 5.0% cosmetics, C adds as adding the cosmetics of 10% bark extract of the Terminalia arjuna tree by embodiment tri-preparations lipid nanoparticle emulsion.
As can be known by Table A, smeared the Terminalia arjuna tree bark extract lipid nanoparticle emulsion that contains embodiment tri-preparation (cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%), this arm skin is obviously than directly adding the 5.0%(mass ratio) cosmetics of Terminalia arjuna tree bark extract and the hydration rate that blank is organized high, illustrate that lipid nanoparticle emulsion moisture-keeping efficacy prepared by the present invention is remarkable.
2, horny layer moisture loss test: sample adopts cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%), the cosmetics that directly add 5.0% Terminalia arjuna tree bark extract and the blank group cosmetics that add 10% bark extract of the Terminalia arjuna tree by embodiment tri-preparations lipid nanoparticle emulsion.
This method of testing is carried out according to the method that provides as Publication about Document: " foundation of cosmetic industry evaluation methodology ", Beijing daily use chemicals, the 4th phase in 2006,20-23 page, Zhao Hua, Dong Yinmao, He Congfen, Lan Sheyi, Wang Changtao.
The assay method of moisture percutaneous lost (TEWL): test philosophy is to close on according to the diffusion principle measurement that A.Fick found in 1885 variation that the skin surface moisture vapor is pressed.Use the circular cylindrical cavity measuring probe of the both ends open of particular design to form metastable test subenvironment at skin surface, by two groups of temperature-humidity sensors, measure the water vapor pressure gradient 2 of differences that nearly epidermis (in about 1cm) is formed by the horny layer moisture loss, directly measure the water quantities through the epidermis evaporation, with this, weigh skin surface water loss situation, thereby can estimate the moisture-keeping efficacy of cosmetics at skin surface.The TEWL value is an important symbol of skin barrier quality, and the TEWL value of skin is lower, illustrates that the barrier function of skin is just better, otherwise poorer.Tewameter carrys out the barrier function of evaluating skin to moisture from skin surface water loss rate, and then estimates the moistening effect of cosmetics.
Experimental technique: measure moisture with Tewameter TM300 moisture of skin loss tester and scatter and disappear (transepidermal water loss is called for short TEWL) through skin.Not direct representation of the TEWL horny layer water yield, it reflects cuticular barrier function, is the important factor of estimating the horny layer state.With formula (2), calculate percutaneous moisture loss rate.
Moisture loss rate=(test value-blank value)/blank value (2)
This experimental result table as shown in the table B
B is as can be known by table, the arm skin of cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%) of smearing the Terminalia arjuna tree bark extract lipid nanoparticle emulsion that is added with embodiment tri-preparation is obviously strong than the ability of the cosmetics that directly add 5.0% Terminalia arjuna tree bark extract and the tested skin surface moisture loss of blank group cosmetics inhibition, namely strengthened the barrier function of skin surface, illustrated that lipid nanoparticle emulsion moisture-keeping efficacy prepared by the present invention is remarkable.
3, crease-resistant efficacy detection: cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%), the cosmetics that directly add 5.0% Terminalia arjuna tree bark extract and the blank group cosmetics that add 10% bark extract of the Terminalia arjuna tree by embodiment tri-preparations lipid nanoparticle emulsion are adopted in 30 routine human body double blind experimenies, sample.
This method of testing adopts the German CK wrinkle of skin tester SV600 of company test wrinkle depth, adopts the VISIA CR of U.S. CANFIELD company to measure whole skin smoothness.
Use the cosmetics that add functional component to detect afterwards the situation of change of wrinkle depth variation and whole skin smoothness in 28 days, experimental data is as follows: table C
Annotate: the blank group of A, B directly adds the cosmetics of 5.0% Terminalia arjuna tree bark extract, and it is the cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%) of 10% bark extract of the Terminalia arjuna tree by embodiment tri-preparations lipid nanoparticle emulsion that C adds.
C is as can be known by table, and the skin of the cosmetics of the Terminalia arjuna tree bark extract lipid nanoparticle emulsion that is added with embodiment tri-preparations of smearing is obviously remarkable than the anti-wrinkle effect of the cosmetics that directly add Terminalia arjuna tree bark extract and blank group cosmetics.
By liquid chromatograph, can measure main mark active matter arjunolic acid.The alcoholic solution of 5% Terminalia arjuna tree bark extract, preserved three months under 45 ℃ of environment, wherein residual arjunolic acid is 66.5% of former content.Preparation becomes and contains 5% Terminalia arjuna tree bark extract lipid nanoparticle emulsion, under 45 ℃ of environment, preserves three months, and residual arjunolic acid is 97.3% of former content.Therefrom can find out by being prepared into nano-lipid grain emulsion, effective prolection thing, in lipid nanoparticle emulsion prepared by the inventive method, contained active matter is very stable.It is simple and convenient that this method also has preparation process, constant product quality, and large-scale industrial is produced convenient grade for beneficial effect.
For the long preservation purpose, the present invention can add a small amount of antiseptic, avoids microbial contamination.
In sum, the inventive method has the following advantages: the Terminalia arjuna tree bark extract lipid nanoparticle good emulsion stability that makes, bioavailability is improved, and moisturizing and anti-wrinkle effect are remarkable in cosmetic formulations, facilitates cold joining to join in cosmetic formulations.
The percentage ratio that designs in the present invention, be mass percent if no special instructions.
The specific embodiment
Embodiment mono-:
A kind of preparation method of Terminalia arjuna tree bark extract lipid nanoparticle emulsion, comprise the steps:
A. take 1g Terminalia arjuna tree bark extract dry powder, add 2g 1, the 2-pentanediol dissolves, and obtains Terminalia arjuna tree bark extract alcoholic solution (mixture A);
B. take 0.5g PLURONICS F87,0.5g poloxamer188,5.0g Natrulon H-10 myristinate, 20.0g stearic acid monoglycerides, A mixes with mixture, then be heated to 75 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirred 10 minutes, obtain the liquid oil phase (mixture B) of homogeneous;
C. take distilled water 71.0g, distilled water is mixed with mixture B, obtain mixed liquor, be heated to 85 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stir, obtain premixed solution (mixture C);
D. mixture C is poured into to high pressure homogenizer emulsifying, controlled pressure is at 70MPa, and temperature is at 85 ℃, and circulation homogenizing 10 times, be cooled to room temperature, obtains the Terminalia arjuna tree bark extract lipid nanoparticle emulsion that the nanoparticle mean diameter is about 150nm.
In the present embodiment gained Terminalia arjuna tree bark extract lipid nanoparticle emulsion, the ratio of each composition is as follows:
Terminalia arjuna tree bark extract 1.0%, 1,2-pentanediol 2.0%, emulsifying agent 6.0% (wherein PLURONICS F87, poloxamer188, Natrulon H-10 myristinate ratio are 0.10: 0.10: 1); Liquid oil phase 29.0 %; Distilled water 71.0%.
As the needs long preservation, can add appropriate antiseptic.
Embodiment bis-:
A kind of preparation method of Terminalia arjuna tree bark extract lipid nanoparticle emulsion, comprise the steps:
A. take 3g Terminalia arjuna tree bark extract dry powder, add 3g 1, the 2-pentanediol dissolves, and obtains Terminalia arjuna tree bark extract alcoholic solution (mixture A);
B. take 0.6g PLURONICS F87,0.7g poloxamer188,3.7g Natrulon H-10 myristinate, 25.0g stearic acid monoglycerides, A mixes with mixture, then be heated to 75 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirred 10 minutes, obtain the liquid oil phase (mixture B) of homogeneous;
C. take the distilled water 64.0g of 85 ℃, distilled water is mixed with mixture B, obtain mixed liquor, with the rotating speed of propeller agitator with 650 rev/mins, mixed liquor is stirred, obtain premixed solution (mixture C);
D. mixture C is poured into to high pressure homogenizer emulsifying, controlled pressure is at 70MPa, and temperature is at 85 ℃, and circulation homogenizing 10 times, be cooled to room temperature, obtains the Terminalia arjuna tree bark extract lipid nanoparticle emulsion that the nanoparticle mean diameter is about 120nm.
In the present embodiment gained Terminalia arjuna tree bark extract lipid nanoparticle emulsion, the ratio of each composition is as follows:
Terminalia arjuna tree bark extract 3.0%, 1,2-pentanediol 3.0%, emulsifying agent 5.0% (wherein PLURONICS F87, poloxamer188, Natrulon H-10 myristinate ratio are 0.162: 0.189: 1); Liquid oil phase 36.0 %; Distilled water 64.0%.
Embodiment tri-:
A kind of preparation method of Terminalia arjuna tree bark extract lipid nanoparticle emulsion, comprise the steps:
A. take 6g Terminalia arjuna tree bark extract dry powder, add 8g 1, the 2-pentanediol dissolves, and obtains Terminalia arjuna tree bark extract alcoholic solution (mixture A);
B. take 2.0g PLURONICS F87,2.0g poloxamer188,4.0g Natrulon H-10 myristinate,
28.0g stearic acid monoglycerides, A mixes with mixture, then is heated to 80 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirs 10 minutes, obtains the liquid oil phase (mixture B) of homogeneous;
C. take the distilled water 50g of 80 ℃, distilled water is mixed with mixture B, obtain mixed liquor, with the rotating speed of propeller agitator with 650 rev/mins, stir, obtain premixed solution (mixture C);
D. mixture C is poured into to high pressure homogenizer emulsifying, controlled pressure is at 100MPa, and temperature is at 80 ℃, and circulation homogenizing 15 times, be cooled to room temperature, obtains the Terminalia arjuna tree bark extract lipid nanoparticle emulsion that the nanoparticle mean diameter is about 80nm.
In the present embodiment gained Terminalia arjuna tree bark extract lipid nanoparticle emulsion, the ratio of each composition is as follows:
Terminalia arjuna tree bark extract 6.0%, 1,2-pentanediol 8.0%, emulsifying agent 8% (wherein PLURONICS F87, poloxamer188, Natrulon H-10 myristinate ratio are 0.50: 0.50: 1); Liquid oil phase 50%; Distilled water 50%.
Embodiment tetra-:
A kind of preparation method of Terminalia arjuna tree bark extract lipid nanoparticle emulsion, comprise the steps
A. take 8g Terminalia arjuna tree bark extract dry powder, add 16g1, the 2-pentanediol dissolves, and obtains Terminalia arjuna tree bark extract alcoholic solution (mixture A);
B. take 3.0g PLURONICS F87,3.0g poloxamer188,4.0g Natrulon H-10 myristinate,
30.0g stearic acid monoglycerides, mix with the compound anti-acne active matter of steps A gained, then is heated to 80 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirred 10 minutes, obtains the liquid oil phase (mixture B) of homogeneous;
C. take the distilled water 36g of 80 ℃, distilled water is mixed with mixture B, obtain mixed liquor, with the rotating speed of propeller agitator with 650 rev/mins, mixed liquor is stirred, obtain premixed solution (mixture C);
D. mixture C is poured into to high pressure homogenizer emulsifying, controlled pressure is at 100MPa, and temperature is at 80 ℃, and circulation homogenizing 15 times, be cooled to room temperature, obtains the Terminalia arjuna tree bark extract lipid nanoparticle emulsion that the nanoparticle mean diameter is about 80nm.
In the present embodiment gained Terminalia arjuna tree bark extract lipid nanoparticle emulsion, the ratio of each composition is as follows:
Terminalia arjuna tree bark extract 8%, 1,2-pentanediol 16.0%, emulsifying agent 10% (wherein PLURONICS F87, poloxamer188, Natrulon H-10 myristinate ratio are 0.75: 0.75: 1); Liquid oil phase 64%; Distilled water 36%.
Claims (1)
1. the preparation method of Terminalia arjuna tree bark extract lipid nanoparticle emulsion is characterized in that comprising the following steps:
A: for the ratio of 0.5-1.0:1.0, Terminalia arjuna is set to bark extract dry powder in mass ratio and be dissolved in 1, the 2-pentanediol dissolves, and obtains Terminalia arjuna tree bark extract alcoholic solution;
B: be 0.15-0.80: 0.20-0.33 in mass ratio: 1 ratio, taking steps A gained Terminalia arjuna tree bark extract alcoholic solution, emulsifying agent and stearic acid monoglycerides mixes, mixed liquor is heated to 75-85 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirred 10 minutes, obtain the liquid oil phase of homogeneous; Described emulsifying agent is the mixture of PLURONICS F87, poloxamer188 and Natrulon H-10 myristinate, and in mixture, three's mass ratio is 0.10-0.75:0.10-0.75:1;
C: be in mass ratio 0.41-1.78: 1 ratio takes step B gained liquid oil phase and distilled water, mixes post-heating to 75-85 ℃, with the rotating speed of propeller agitator with 650 rev/mins, stirs, and obtains premixed solution;
D: step C gained premixed solution, under 75-85 ℃ of temperature conditions, 70-150MPa pressures cycle homogenizing 8-15 times, is cooled to room temperature by high pressure homogenizer, obtains Terminalia arjuna tree bark extract lipid nanoparticle emulsion.
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