CN103202784B - Preparation method of common bombax flower extract with whitening and anti-aging activities, and application thereof in cosmetics - Google Patents
Preparation method of common bombax flower extract with whitening and anti-aging activities, and application thereof in cosmetics Download PDFInfo
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- CN103202784B CN103202784B CN201210114034.4A CN201210114034A CN103202784B CN 103202784 B CN103202784 B CN 103202784B CN 201210114034 A CN201210114034 A CN 201210114034A CN 103202784 B CN103202784 B CN 103202784B
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- bombacis malabarici
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Abstract
The invention discloses a preparation method of a common bombax flower extract with whitening and anti-aging activities. The preparation method is characterized in that dried common bombax flowers are crushed and sieved; the common bombax flower is subjected to ethanol soaking extraction twice; extracted liquids obtained in the two times are combined; reduced-pressure concentration is carried out, such that a suspension liquid is obtained; the suspension liquid is sequentially extracted by using petroleum ether and ethyl acetate; reduced-pressure concentration is carried out, and ethyl acetate is recovered; and a paste is obtained by vacuum drying, such that the common bombax flower extract is obtained. With the method, the prepared common bombax flower extract has anti-free radical oxidation, tyrosinase activity inhibiting, and anti-ultraviolet radiation functions, and can be used in skin whitening and aging-preventing especially photoaging-preventing. The common bombax flower extract can be used as a cosmetic additive or a medicine active component, and can be applied in whitening and anti-aging cosmetics.
Description
Technical field
The present invention relates to the preparation method of Flos Bombacis Malabarici extract, this extract has whitening and senile-resistant efficacy, can be applied to whitening anti-aging cosmetics, belongs to field of fine chemical.
Background technology
Skin-whitening defying age is the theme of cosmetics, and the cosmetics with skin-whitening anti-senescence function are one of main flow cosmetics of consumer's favor.Modern scientific research proves, skin aging is a very complicated process, is subject to the impact of many factors, and wherein melanic generation and free radical cause that the degeneration of elastic fibers of skin is two large principal elements.
The color of human skin depends on melanic content and distribution, inhomogeneous in human body deposition distribution when a large amount of melanin, will form freckle, chloasma.Tryrosinase is extensively present in human body, is to produce melanic key enzyme.Melanic forming process is: the tyrosine in human body skin melanocyte is oxidized generation DOPA and DOPA quinone under the catalytic action of tryrosinase, generate dopachrome, 5 through resetting laggard oxidation step, 6-dihydroxy indole, istain, final synthesis of melanin.At present the dominant mechanism of conventional whitening agent cosmetics is active by restraint of tyrosinase or the oxidation of blocking-up tyrosine generates melanin, thereby reduces melanic generation and reach the effect of skin-whitening.
Free radical is the key factor that causes skin aging, and air pollution, pressure, medicine etc. all can make health produce free radical, and ultraviolet is the main source of skin free radical.The molecule that free radical contains one or more unpaired electrons or a part for molecule, have the tendency of pairing.Therefore most of free radicals are all very active, have the chemism of height.Under normal circumstances, the free radical in human body is among the dynamic equilibrium in continuous generation and removing.But free-radical generating too much or removed slowly, and it,, by attacking life macromolecule material and various cell, can cause the various damages of body, accelerates the senescence process of body, shows old and feeble gradually variation, as age pigment deposits, skin is wrinkling etc.Therefore,, in whitening, strengthen free radical resisting extremely important.
Now, skin-lightening cosmetic market development is very rapid, and the developmental research of whitening agent is also constantly released.In recent years, the whitening agent using in cosmetics mainly contains the compounds such as hydroquinone (hydroquinone), L-AA (vitamin C), kojic acid and arbutin.But these whitening agents exist many defects, as the zest of hydroquinone is very large, vitamin C is very unstable, and kojic acid is unstable to light, heat and metal ion, and skin absorption is poor, the single and poor effect of arbutin effect etc.So exploitation has good safety, stability, inhibition is obvious, and the natural whiting agent that cost performance is good, has become one of main direction of studying of current medicine and cosmetic industry, has extraordinary development prospect.
Flos Bombacis Malabarici common bombax flower is the dried floral of Bombacaceae plant kapok Bombax malabaricum (DC.) Merr, another name Flos Bombacis Malabarici, speckle sesame.Be distributed in the provinces and regions such as southern Guangdong, Guangxi, Yunnan, Sichuan, Hainan, Fujian, Taiwan.Begin to be loaded in clearly what gram remonstrate with " the SHENGCAO property of medicine is standby to be wanted ".Nature and flavor are sweet, cool.There is effect of clearing away heat-damp and promoting diuresis, removing toxic substances and hemostasis.Cure mainly enteritis, have loose bowels, bleeding hemorrhoids, bacillary dysentery.Flos Bombacis Malabarici is usually used in Chinese medicine compound, as golden aster five-flower tea granule, for having loose bowels due to damp-heat in the large intestine, dysentery, have blood in stool, hemorrhoidal bleeding and liver-heat conjunctival congestion, wind heat pharyngalgia, dispute is festered etc.
At present, the research to Flos Bombacis Malabarici and application deepen continuously.Research shows, Flos Bombacis Malabarici containing volatile ingredient as hexadecanoic acid, ethyl palmitate, Ethyl linoleate etc.; Triterpenes components is as lupeol, lupenone etc.; Flavone compound is as aromadendrin, Quercetin, luteolin etc.But the application of Flos Bombacis Malabarici is mostly in industries such as food, medicine, health cares, and the research in cosmetics is also little for it, and the research being especially applied in whitening anti-aging cosmetics there is not yet report.Due to the recyclability of plant, develop Flos Bombacis Malabarici to obtain better active component, be an important opportunity of present cosmetics scientific research and innovation.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the Flos Bombacis Malabarici extract with whitening anti-aging activity, this Flos Bombacis Malabarici extract has effect of free radical resisting oxidation, restraint of tyrosinase activity and ultraviolet radiation resisting.
The preparation scheme of Flos Bombacis Malabarici extract of the present invention is as follows:
1. dry Flos Bombacis Malabarici is made to powder, cross 40～80 mesh sieves;
2. Flos Bombacis Malabarici powder is put into round-bottomed flask, add 5mL～30mL alcoholic solution (in alcoholic solution, the mass concentration of ethanol is between 30%～80%) by every 1g Flos Bombacis Malabarici powder, then under 40 DEG C～80 DEG C conditions, adding heat soaking extracts twice, each 1h～3h that extracts, merge extracted twice liquid, obtain crude extract;
3. Flos Bombacis Malabarici ethanol crude extract concentrating under reduced pressure is reclaimed to ethanol, obtain suspension;
4. use petroleum ether extraction suspension, described petroleum ether mixes with suspension for 3: 1 by volume, 2: 1 or 1: 1, removes pigment and tannin, obtains refining liquid;
5. be extracted with ethyl acetate the active substance in refining liquid, described ethyl acetate is mixed with refining liquid for 3: 1 by volume, 2: 1 or 1: 1, and concentrating under reduced pressure becomes mastic by activity extract vacuum drying after reclaiming ethyl acetate.
Another object of the present invention be by Flos Bombacis Malabarici extract for whitening anti-aging cosmetics, make stable in properties, respond well whitening anti-aging cosmetics.The dosage form of whitening anti-aging cosmetics is not particularly limited, and can be solution, emulsion, paste, powdery etc.
The invention has the beneficial effects as follows by test, uv absorption, the oxidation of anti-hydroxy radical and the human trial of the inhibitory action to tryrosinase, melanocyte and verify that Flos Bombacis Malabarici extract has skin-whitening and senile-resistant efficacy.
Detailed description of the invention
Come by specific embodiment below that the present invention is further illustrated, but these embodiment are just in order to illustrate, are not limitations of the present invention.
Embodiment 1 has the preparation of the Flos Bombacis Malabarici extract of whitening anti-aging activity
Accurately take dried Flos Bombacis Malabarici 50g under natural environment, be ground into particle mean size at 50 object powder; The ethanol water that is 70% with 750mL mass concentration by Flos Bombacis Malabarici powder mixes, and adds in round-bottomed flask, then with 80 DEG C of water-bath lixiviate 1.5h twice, merges extracted twice liquid, obtains crude extract; By the Flos Bombacis Malabarici ethanol crude extract concentrating under reduced pressure obtaining, reclaim ethanol, obtain suspension; Petroleum ether and suspension are extracted for 2: 1 by volume, combining extraction liquid, concentrating under reduced pressure reclaims petroleum ether, obtains refining liquid; Ethyl acetate and refining liquid are extracted to ethyl acetate layer in 2: 1 by volume substantially colourless, combining extraction liquid, concentrating under reduced pressure reclaims ethyl acetate, and active component dry 18h in the vacuum drying oven of 50 DEG C is obtained to extractum.
Embodiment 2 restraint of tyrosinase active testings
(1) material
1. solution preparation
(1) HCl (0.1mol/L): the hydrochloric acid solution of 0.862mL 36%～38% is dissolved in 99.138mL water.
(2) TYR solution: 0.05g is dissolved in the HCl of 35mL 0.1mol/L, is settled to 100mL with PBS (0.1mol/L) buffer of pH6.8.
(3) PBS solution (pH=6.8,0.1mol/L): 1. 17.91g disodium hydrogen phosphate is dissolved in deionized water, is settled to 500mL with deionized water.2. 7.8g ten sodium dihydrogen phosphate dihydrates are dissolved in deionized water, are settled to 500mL with deionized water.3. get respectively 92.6mL and 107.4mL and be mixed with the phosphate buffer solution of 200mLpH=6.8.
(4) tryrosinase: 100U/mL.
2. sample preparation
Above-mentioned Flos Bombacis Malabarici extract is dissolved in dimethyl sulfoxine, is made into concentration and is 0.1% sample solution, carry out test below.Simultaneously with arbutin sample in contrast.
(2) instrument
10mL test tube, water-bath, agitator.
(3) test method
1. according to table 1 application of sample, do not add tryrosinase.Arbutin is contrasted as one group of sample.
Table 1
2. solution is placed in to 37 DEG C of water-bath constant temperature 10min.
3. add tryrosinase, solution is placed in after 37 DEG C of water-bath constant temperature 10min, under 475nm, measure its absorbance, and compare with arbutin.
Tyrosinase activity suppression ratio calculates according to formula (1):
Tyrosinase activity suppression ratio=(blank absorbency value-sample absorbance)/blank absorbency value × 100 (1)
Melanin synthetic test in embodiment 3 check melanin cells
B16 melanoma cell is inoculated in 96 orifice plates to every hole 90 μ L, CO with the density of 1 × 105/mL
2in incubator, hatch after 24 hours, every hole adds sample solution.Set up the blank group of culture medium and cell simultaneously.
Culture plate is placed in to incubator and hatches after 72 hours, abandoning supernatant, PBS washing twice, then every hole adds 0.5mL trypsin digestion cell 3min, and every hole adds 2mL maintenance medium to stop digestion.After mixing, every kind of concentration is taken out 0.5mL and is made cell counting.All the other cell suspension are with 2500r/min centrifugalize 5min, and abandoning supernatant adds NaOH solution in precipitation, and heating is dissolved melanin, select 490nm wavelength to measure absorbance under enzyme-linked immunosorbent assay instrument.By formula (2) calculation sample to the synthetic suppression ratio of melanin (I ').
The anti-hydroxyl radicals of embodiment 4 salicylic acid method test active matter
(1) test principle
In system, reacting by Fenton the OH oxidation salicylic acid generation producing has 2 of special absorption to 510nm light, 3-dicarboxyl benzoic acid, and the product obtaining by mensuration capture by salicylic acid OH is determined the clearance rate of OH.Reaction equation is: H
2o
2+ Fe
2+→ OH+OH
-+ Fe
3+
(2) material
1. reagent: salicylic acid, FeSO
4, H
2o
2
2. sample: by soluble in water Flos Bombacis Malabarici extract extractum, be made into concentration and be 0.1% sample solution, and with the arbutin of same concentrations in contrast.
3. instrument: 25mL test tube, water-bath, ultraviolet spectrophotometer, 1mL, 5mL liquid-transfering gun.
(3) test method
In 25mL color comparison tube, add successively 2mmol/L FeSO
43mL, 1mmol/L H
2o
23mL, shakes up, and then adds 6mmol/L salicylic acid 3mL, shakes up, and after 37 DEG C of heating in water bath 15min, takes out, and surveys its absorbance A
o.Then add respectively certain density liquid 0.2mL to be measured, 0.4mL, 0.6mL, 0.8mL, 1.0mL, and then add respectively distilled water 0.8mL, 0.6mL, 0.4mL, 0.2mL, 0mL, shake up, continue heating in water bath 15min, take out and survey its absorbance A
x.As stated above, add each liquid as shown in table 2, do not add salicylic acid, shake up, heating in water bath 15min, measured value A
xo.Calculate free radical scavenging activity by formula (3).
The free clearance rate of hydroxyl (%)=A
o-(A
x-A
xo)/A
o* 100 (3)
A
o---the light absorption value of blank
A
x---add the light absorption value of sample
A
xo---do not add developer H
2o
2solution background absorption value
Table 2
Embodiment 5 uvioresistant effect assessment tests
Test according to the light industry standard QB/T 2334-1997 of the People's Republic of China (PRC) (cosmetics middle-ultraviolet lamp absorbent qualitative determination-ultraviolet spectrophotometry).Sample extractum is dissolved in 95% ethanol, is made into concentration and is 0.1% sample solution, then, within the scope of 280～400nm, scan every 10nm, determine the absorbance under each wavelength, and calculate mean light absorbency.
Table 3 has provided the whitening and skin-protecting effect assessment experimental result of Flos Bombacis Malabarici extract.
Table 3 whitening and skin-protecting effect assessment experimental result
Find by above every whitening and skin-protecting evaluation experimental, Flos Bombacis Malabarici extract of the present invention is synthesizing of the active and check melanin of restraint of tyrosinase effectively, have the hydroxy radical of removing and anti-ultraviolet function, these functions are all better than conventional arbutin whitening agent at present simultaneously.
Embodiment 6 human body whitenings are evaluated
(1) principle
Utilize three kinds of different wave lengths to absorb and reflect the amount to measure melanin and haemachrome, determining the performance of skin color.
(2) test sample and object
Flos Bombacis Malabarici extract extractum is added in the conventional emulsifiable paste without whitening effect by 3% addition, as test sample.Select the age be 18 years old～50 years old healthy volunteer without dermatosis and allergies as tested object, volunteer's number 10 people, each 5 people of men and women.
(3) test instrunment
Mexamter MX18 (CK Electronic GmH, Germany)
(4) test condition
Room temperature is below 20 ± 2 DEG C, and relative humidity (RH) is below 50 ± 5%; Testee 30min before mensuration enters in test environment quiet to be measured, and before mensuration, 10min exposes tested position.
(5) method
According to test request, choose testee's facial left and right cheek and the front wrist of right arm and bend the suitable area in lateral areas as Bei Yan district.Before makeup application, by the probe vertical of Mexamter MX18 be placed on skin, after 3s～5s, after value stabilization to be determined, read melanin and the red pigment numerical value at tested position.Measure respectively melanin and red pigment numerical value instant after makeup application, after 1 week, 2 weeks, 3 weeks, 4 weeks, 5 weeks, 6 weeks according to standardization program; Respectively tested the dark red pigment at position and got mensuration 5 times, got its meansigma methods.
(6) result of the test
Experimental result is in table 4 and table 5.
The melanin value of table 4 use test sample different time
The red pigment value of table 5 use test sample different time
This test represents the color of skin with dermal melanin and red pigment content, melanin and the fewer skin color of red pigment content are more shallow, whiter.Can be found out by table 4 and table 5, Flos Bombacis Malabarici extract adds in the conventional emulsifiable paste without whitening effect, has obvious whitening effect.
The preparation of embodiment 7 body whitening crème
Table 6 provides the body whitening crème formula that contains Flos Bombacis Malabarici extract, and the consumption of each material represents with mass fraction.
Table 6
The preparation method of body whitening crème: A component is mixed, be heated to 75 DEG C, thawing stirs, and adds B component before emulsifying.C component (except Flos Bombacis Malabarici extract) is mixed and heated to 75 DEG C, under stirring, A component and B component are slowly added in C component, homogenizing processing, in the time being cooled to 50 DEG C, add Flos Bombacis Malabarici extract and D component, continue slowly to stir, be cooled to room temperature, after ageing 24h, can pack.
The preparation of embodiment 8 whitening and skin-protecting breasts
Table 7 provides the whitening and skin-protecting breast formula that contains Flos Bombacis Malabarici extract, and the consumption of each material represents with mass fraction.
Table 7
The preparation method of whitening and skin-protecting breast: each A component material (except Flos Bombacis Malabarici extract) is added to the water, is heated to 85 DEG C it is dissolved, make water.Separately B component is mixed to post-heating to 85 DEG C melting, add C component before emulsifying, dispersed with stirring evenly makes oil phase.Under stirring, B component and C component are slowly added in A component, homogenizing processing adds Flos Bombacis Malabarici extract and D component in the time being cooled to 50 DEG C, continues slowly to stir, and is cooled to room temperature, after ageing 24h, can pack.
Claims (1)
1. Flos Bombacis Malabarici extract is in the purposes of preparing in whitening anti-aging cosmetics, it is characterized in that described Flos Bombacis Malabarici extract prepared according to following steps:
(1) dry Flos Bombacis Malabarici is made to powder, cross 40～80 mesh sieves;
(2) Flos Bombacis Malabarici powder is put into round-bottomed flask, add 5mL～30mL alcoholic solution by every 1g Flos Bombacis Malabarici powder, in described alcoholic solution, the mass concentration of ethanol is between 30%～80%, then under 40 DEG C～80 DEG C conditions, adding heat soaking extracts twice, each 1h～3h that extracts, merge extracted twice liquid, obtain crude extract;
(3) Flos Bombacis Malabarici ethanol crude extract concentrating under reduced pressure is reclaimed to ethanol, obtain suspension;
(4) use petroleum ether extraction suspension, described petroleum ether mixes with suspension for 3: 1 by volume, 2: 1 or 1: 1, removes pigment and tannin, obtains refining liquid;
(5) be extracted with ethyl acetate the active substance in refining liquid, described ethyl acetate is mixed with refining liquid for 3: 1 by volume, 2: 1 or 1: 1, and concentrating under reduced pressure becomes mastic by activity extract vacuum drying after reclaiming ethyl acetate.
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| CN106924109A (en) * | 2017-02-15 | 2017-07-07 | 玉林祺钟商贸有限公司 | A kind of whitening skin care product |
| CN107714570B (en) * | 2017-12-08 | 2020-05-19 | 玮格沃德贸易有限公司 | Plant extract, preparation method and application thereof in cosmetics |
| FR3075642B1 (en) * | 2017-12-22 | 2021-10-22 | Expanscience Lab | KAPOKIER FLOWER EXTRACT AND COSMETIC, PHARMACEUTICAL OR DERMATOLOGICAL COMPOSITIONS CONTAINING IT |
| CN110763597A (en) * | 2019-07-31 | 2020-02-07 | 杭州曼迪生物科技有限公司 | Method for evaluating whitening effect of cosmetics based on transdermal absorption |
| CN112156119B (en) * | 2020-11-09 | 2023-04-28 | 广东丸美生物技术股份有限公司 | Application of kapok alcohol extract and medicament for inhibiting propionibacterium acnes |
| CN114469815A (en) * | 2022-02-25 | 2022-05-13 | 广东丸美生物技术股份有限公司 | Common bombax flower extract and preparation method and application thereof |
| CN114931535B (en) * | 2022-06-29 | 2023-09-26 | 广东远宸医药生物科技有限公司 | Preparation method and application of kapok extract with moisturizing and relieving effects |
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| CN1506108A (en) * | 2002-12-09 | 2004-06-23 | 戚海燕 | Composite milk powder capable of being eaten and made into beautifying face mask |
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| CN1506108A (en) * | 2002-12-09 | 2004-06-23 | 戚海燕 | Composite milk powder capable of being eaten and made into beautifying face mask |
Non-Patent Citations (1)
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| 王辉，等.木棉花醇提物中乙酸乙酯溶解组分的化学成分研究.《林产化学与工业》.2004,第24卷(第2期),第89-91页. * |
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Address after: 510663 No. 15, Colin Road, Guangzhou Science City, Guangzhou high tech Industrial Development Zone, Guangdong Province Patentee after: Guangzhou Huanya cosmetics technology Co.,Ltd. Address before: 510663 No. 15, Colin Road, Guangzhou Science City, Guangzhou high tech Industrial Development Zone, Guangdong Province Patentee before: GUANGZHOU HUANYA COSMETICS TECHNOLOGY Co.,Ltd. |
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