CN103393580B - Preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion - Google Patents
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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 liposome technology field, particularly a kind of preparation method of Terminalia arjuna bark extract lipid nanoparticle emulsion.
Background technology
Active component mainly multiple olive alkanes triterpenoid in Terminalia arjuna tree bark extract (INCI title: TERMINALIA ARJUNA), and wherein the most important thing is arjunolic acid (Arjunolic acid).Commercial Terminalia arjuna has been had to set bark extract at present, arjunolic acid (Arjunolic acid) wherein containing 80% purity, it is pentacyclic triterpenoid, and other 20% mainly some tannins and Flavonoid substances, manufacturer is SABINSA company of the U.S..Research finds that Terminalia arjuna tree bark extract has stronger antiinflammatory and antidotal effect, by strengthening skin blood microcirculation, increase skin elasticity and dermis density, contribute to recovering the natural sebum levels of skin after climacteric and skin barrier performance can be strengthened, make skin become more smooth, be applied in cosmetic formulations application and show obvious moisturizing and crease-resistant effect.Terminalia arjuna tree bark extract is alcohol soluble substance, and it is less stable in cosmetic formulations, and bioavailability is low, easy oxidized variable color.Due to this characteristic of Terminalia arjuna tree bark extract in prior art, cause it in the being greatly limited property of scope of application.Terminalia arjuna is set bark extract and is prepared into lipid nanoparticle emulsion, add in cosmetic formulations, its stability, range of application, bioavailability can be made to be improved.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of preparation method of lipid nanoparticle emulsion of energy load Terminalia arjuna tree bark extract; 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, making Terminalia arjuna set bark extract is not easy oxidized, 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: a kind of preparation method of Terminalia arjuna bark extract lipid nanoparticle emulsion, is characterized in that comprising the following steps:
A: Terminalia arjuna is set bark extract dry powder for the ratio of 0.5-1.0:1.0 in mass ratio and be dissolved in 1,2-pentanediol and dissolve, obtain Terminalia arjuna tree bark extract alcoholic solution;
B: be the ratio of 0.15-0.80: 0.20-0.33: 1 in mass ratio, take steps A gained Terminalia arjuna tree bark extract alcoholic solution, emulsifying agent and stearic acid monoglycerides to mix, mixed liquor is heated to 75-85 DEG C, stir 10 minutes with propeller agitator with the rotating speed of 650 revs/min, obtain homogeneous liquid oil phase; Described emulsifying agent is the mixture of PLURONICS F87, poloxamer188 and Natrulon H-10 myristinate, and in mixture, the mass ratio of three is 0.10-0.75:0.10-0.75:1;
C: in mass ratio for the ratio of 0.41-1.78: 1 takes step B gained liquid oil phase and distilled water, mixing post-heating, to 75-85 DEG C, stirs with the rotating speed of 650 revs/min with propeller agitator, obtains premixed solution;
D: by step C gained premixed solution under 75-85 DEG C of temperature conditions, by high pressure homogenizer 70-150MPa pressures cycle homogenizing 8-15 times, is cooled to room temperature, obtains Terminalia arjuna bark extract lipid nanoparticle emulsion.
By Terminalia arjuna bark extract lipid nanoparticle emulsion prepared by the inventive method, comprise the Terminalia arjuna tree bark extract that mass percent is 1.0-8.0%.
By Terminalia arjuna bark extract lipid nanoparticle emulsion prepared by the inventive method, under room temperature, viscosity is less than 1000cps, is easy to topple over, and coldly can join and join in cosmetic formulations, as active additive in moisturizing and crease-resistant both effectiveness cosmetics, use easily; Terminalia arjuna bark extract lipid nanoparticle emulsion prepared by the inventive method is that in the centrifuge of 10000 turns per minute, centrifugal 30min is not stratified at rotating speed; Invariant color in three months is preserved under 45 DEG C of environment, not stratified.Keep 3 years under room temperature, invariant color, not stratified.
Nanoparticle particle diameter in Terminalia arjuna bark extract lipid nanoparticle emulsion prepared by the present invention can control within the scope of 65-150nm, have particle diameter little, be easy to infiltration, stability and bioavailability thereof are improved, and facilitate coldly to join the advantage joined in cosmetic formulations.
Be below the test result of Efficacy experiments of the present invention:
1, keratodermatitis hydration rate test: the cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%) of the Terminalia arjuna bark extract lipid nanoparticle emulsion that sample adopts interpolation 10% to prepare by embodiment three, the cosmetics directly adding 5.0% Terminalia arjuna tree bark extract and blank group cosmetics.
This method of testing is carried out according to the method that such as Publication about Document provides: " 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 take capacitor as instrument probe, because water is the material that on skin, dielectric constant is maximum, when skin moisture content changes, the capacitance of skin also changes, so can by measuring skin pricktest capacitance, analyzing skin surface moisture content.Conventional instrument is Corneometer CM825.By measuring the change using the change of keratodermatitis capacitance before and after product to weigh water content of stratum corneum, thus evaluate the moisture-keeping efficacy of cosmetics, this kind of method carries out quantification to the moisture of keratodermatitis, the change of skin moisture content can be reacted delicately, and favorable reproducibility, be one of method that current moisture-keeping cosmetics efficacy assessments is conventional.
Experimental technique: bend the square Experimental Area that 3 × 3cm2 size is marked in side at candidate left and right forearm, using left arm as the test zone of moisturizer, the corresponding symmetrical region of right arm is blank, then the moisture at each test position is detected with Corneometer CM825 tester, repeat 5 times respectively, draw meansigma methods.By formula (1) calculated hydration rate.
Hydration rate=(test value-blank value)/blank value (1)
Experimental result sees the following form.Table A
The blank group of note: A, the content that B directly adds Terminalia arjuna tree bark extract is the cosmetics of 5.0%, and C adds the cosmetics for adding the Terminalia arjuna bark extract lipid nanoparticle emulsion that 10% prepares by embodiment three.
From Table A, Terminalia arjuna bark extract lipid nanoparticle emulsion (the cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%) prepared containing embodiment three are smeared, this arm skin is obviously than directly adding 5.0%(mass ratio) hydration rate of the cosmetics of Terminalia arjuna tree bark extract and blank group is high, illustrates that lipid nanoparticle emulsion moisture-keeping efficacy prepared by the present invention is remarkable.
2, horny layer moisture loss test: the cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%) of the Terminalia arjuna bark extract lipid nanoparticle emulsion that sample adopts interpolation 10% to prepare by embodiment three, the cosmetics directly adding 5.0% Terminalia arjuna tree bark extract and blank group cosmetics.
This method of testing is carried out according to the method that such as Publication about Document provides: " 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 measures in the diffusion principle that 1885 find the change closing on skin surface moisture vapor pressure according to A.Fick.The circular cylindrical cavity measuring probe of the both ends open of particular design is used to form metastable test subenvironment at skin surface, by two groups of temperature-humidity sensors measure nearly epidermis (about within 1cm) by horny layer moisture loss formed the water vapor pressure gradient of different 2, directly measure the water quantities through epidermis evaporation, weigh skin surface water loss situation with this, thus the moisture-keeping efficacy of cosmetics at skin surface can be evaluated.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 better, otherwise then poorer.Tewameter carrys out the barrier function of evaluating skin to moisture from skin surface water loss rate, and then evaluates the moistening effect of cosmetics.
Experimental technique: measure moisture with Tewameter TM300 skin water loss tester and scatter and disappear (transepidermal water loss is called for short TEWL) through skin.The TEWL not direct representation horny layer water yield, it reflects cuticular barrier function, is the important factor evaluating horny layer state.Percutaneous moisture loss rate is calculated by formula (2).
Moisture loss rate=(test value-blank value)/blank value (2)
This experimental result table as shown in the table B
From table B, the arm skin smearing the cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%) being added with Terminalia arjuna bark extract lipid nanoparticle emulsion prepared by embodiment three obviously suppresses the ability of tested skin surface moisture loss strong than the cosmetics and blank group cosmetics that directly add 5.0% Terminalia arjuna tree bark extract, namely enhance the barrier function of skin surface, illustrate that lipid nanoparticle emulsion moisture-keeping efficacy prepared by the present invention is remarkable.
3, crease-resistant efficacy detection: 30 routine human body double blind experimenies, the cosmetics (in cosmetics, the content of Terminalia arjuna tree bark extract is equivalent to 5.0%) of the Terminalia arjuna bark extract lipid nanoparticle emulsion that sample adopts interpolation 10% to prepare by embodiment three, the cosmetics directly adding 5.0% Terminalia arjuna tree bark extract and blank group cosmetics.
This method of testing adopts German CK company wrinkle of skin tester SV600 to test wrinkle depth, adopts CANFIELD company of U.S. VISIA CR to measure overall skin smoothness.
Use the cosmetics adding functional component within 28 days, to detect the situation of change of wrinkle depth change and overall skin smoothness afterwards, experimental data is as follows: table C
The blank group of note: A, B directly add 5.0% Terminalia arjuna tree bark extract cosmetics, C add be 10% by embodiment three prepare Terminalia arjuna bark extract lipid nanoparticle emulsion cosmetics (in cosmetics Terminalia arjuna tree bark extract content be equivalent to 5.0%).
From table C, the skin being added with the cosmetics of Terminalia arjuna bark extract lipid nanoparticle emulsion prepared by embodiment three smeared is obviously remarkable than the anti-wrinkle effect of the cosmetics and blank group cosmetics that directly add Terminalia arjuna tree bark extract.
Main mark active matter arjunolic acid can be measured by liquid chromatograph.The Terminalia arjuna of 5% sets the alcoholic solution of bark extract, and preserve three months under 45 DEG C of environment, wherein residual arjunolic acid is 66.5% of former content.Prepare the Terminalia arjuna bark extract lipid nanoparticle emulsion become containing 5%, preserve three months under 45 DEG C of environment, residual arjunolic acid is 97.3% of former content.Therefrom can find out by being prepared into nano-lipid grain emulsion, can available protecting active matter, in lipid nanoparticle emulsion prepared by the inventive method, contained active matter is highly stable.It is simple and convenient that this method also has preparation process, constant product quality, and large-scale industrial produces convenient grade for beneficial effect.
For preserving object for a long time, the present invention can add a small amount of antiseptic, avoids microbial contamination.
In sum, the inventive method has the following advantages: obtained Terminalia arjuna bark extract lipid nanoparticle emulsion good stability, bioavailability is improved, and in cosmetic formulations, moisturizing and anti-wrinkle effect significantly, facilitate cold joining to join in cosmetic formulations.
The percentage ratio designed in the present invention, is mass percent if no special instructions.
Detailed description of the invention
embodiment one:
A preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion, comprises the steps:
A. take 1g Terminalia arjuna tree bark extract dry powder, add 2g 1,2-pentanediol and dissolve, obtain Terminalia arjuna tree bark extract alcoholic solution (mixture A);
B. 0.5g PLURONICS F87,0.5g poloxamer188,5.0g Natrulon H-10 myristinate, 20.0g stearic acid monoglycerides is taken, mix with mixture A, then 75 DEG C are heated to, stir 10 minutes with propeller agitator with the rotating speed of 650 revs/min, obtain homogeneous liquid oil phase (mixture B);
C. take distilled water 71.0g, distilled water is mixed with mixture B, obtains mixed liquor, be heated to 85 DEG C, stir with the rotating speed of 650 revs/min with propeller agitator, obtain premixed solution (mixture C);
D. pour mixture C into high pressure homogenizer emulsifying, controlled pressure is at 70MPa, and temperature is at 85 DEG C, and circulation homogenizing 10 times, is cooled to room temperature, obtains the Terminalia arjuna bark extract lipid nanoparticle emulsion that nanoparticle mean diameter is about 150nm.
In the present embodiment gained Terminalia arjuna 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%.
Preservation as long-term in needs, can add appropriate antiseptic.
embodiment two:
A preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion, comprises the steps:
A. take 3g Terminalia arjuna tree bark extract dry powder, add 3g 1,2-pentanediol and dissolve, obtain Terminalia arjuna tree bark extract alcoholic solution (mixture A);
B. 0.6g PLURONICS F87,0.7g poloxamer188,3.7g Natrulon H-10 myristinate, 25.0g stearic acid monoglycerides is taken, mix with mixture A, then 75 DEG C are heated to, stir 10 minutes with propeller agitator with the rotating speed of 650 revs/min, obtain homogeneous liquid oil phase (mixture B);
C. take the distilled water 64.0g of 85 DEG C, distilled water is mixed with mixture B, obtains mixed liquor, with the rotating speed of 650 revs/min, mixed liquor is stirred with propeller agitator, obtain premixed solution (mixture C);
D. pour mixture C into high pressure homogenizer emulsifying, controlled pressure is at 70MPa, and temperature is at 85 DEG C, and circulation homogenizing 10 times, is cooled to room temperature, obtains the Terminalia arjuna bark extract lipid nanoparticle emulsion that nanoparticle mean diameter is about 120nm.
In the present embodiment gained Terminalia arjuna 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 three:
A preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion, comprises the steps:
A. take 6g Terminalia arjuna tree bark extract dry powder, add 8g 1,2-pentanediol and dissolve, obtain 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, mixes with mixture A, is then heated to 80 DEG C, stirs 10 minutes with propeller agitator with the rotating speed of 650 revs/min, obtains homogeneous liquid oil phase (mixture B);
C. take the distilled water 50g of 80 DEG C, distilled water is mixed with mixture B, obtains mixed liquor, stir with the rotating speed of 650 revs/min with propeller agitator, obtain premixed solution (mixture C);
D. pour mixture C into high pressure homogenizer emulsifying, controlled pressure is at 100MPa, and temperature is at 80 DEG C, and circulation homogenizing 15 times, is cooled to room temperature, obtains the Terminalia arjuna bark extract lipid nanoparticle emulsion that nanoparticle mean diameter is about 80nm.
In the present embodiment gained Terminalia arjuna 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 four:
A preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion, comprises the steps
A. take 8g Terminalia arjuna tree bark extract dry powder, add 16g1,2-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, mixes with steps A gained compound anti-acne active matter, is then heated to 80 DEG C, stirs 10 minutes with propeller agitator with the rotating speed of 650 revs/min, obtain homogeneous liquid oil phase (mixture B);
C. take the distilled water 36g of 80 DEG C, distilled water is mixed with mixture B, obtains mixed liquor, with the rotating speed of 650 revs/min, mixed liquor is stirred with propeller agitator, obtain premixed solution (mixture C);
D. pour mixture C into high pressure homogenizer emulsifying, controlled pressure is at 100MPa, and temperature is at 80 DEG C, and circulation homogenizing 15 times, is cooled to room temperature, obtains the Terminalia arjuna bark extract lipid nanoparticle emulsion that nanoparticle mean diameter is about 80nm.
In the present embodiment gained Terminalia arjuna 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. a preparation method for Terminalia arjuna bark extract lipid nanoparticle emulsion, is characterized in that comprising the following steps:
A: Terminalia arjuna is set bark extract dry powder for the ratio of 0.5-1.0:1.0 in mass ratio and be dissolved in 1,2-pentanediol and dissolve, obtain Terminalia arjuna tree bark extract alcoholic solution;
B: be the ratio of 0.15-0.80: 0.20-0.33: 1 in mass ratio, take steps A gained Terminalia arjuna tree bark extract alcoholic solution, emulsifying agent and stearic acid monoglycerides to mix, mixed liquor is heated to 75-85 DEG C, stir 10 minutes with propeller agitator with the rotating speed of 650 revs/min, obtain homogeneous liquid oil phase; Described emulsifying agent is the mixture of PLURONICS F87, poloxamer188 and Natrulon H-10 myristinate, and in mixture, the mass ratio of three is 0.10-0.75:0.10-0.75:1;
C: in mass ratio for the ratio of 0.41-1.78: 1 takes step B gained liquid oil phase and distilled water, mixing post-heating, to 75-85 DEG C, stirs with the rotating speed of 650 revs/min with propeller agitator, obtains premixed solution;
D: by step C gained premixed solution under 75-85 DEG C of temperature conditions, by high pressure homogenizer 70-150MPa pressures cycle homogenizing 8-15 times, is cooled to room temperature, obtains Terminalia arjuna bark extract lipid nanoparticle emulsion.
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| CN113350241B (en) * | 2021-06-30 | 2022-11-08 | 广州市科能化妆品科研有限公司 | Application of Terminalia catappa leaf extract, and allergy-relieving composition and application thereof |
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