CN103385837B - Myrica rubra leaf proanthocyanidin toning lotion and preparation method of myrica rubra leaf proanthocyanidin toning lotion - Google Patents
Myrica rubra leaf proanthocyanidin toning lotion and preparation method of myrica rubra leaf proanthocyanidin toning lotion Download PDFInfo
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- CN103385837B CN103385837B CN201310332090.XA CN201310332090A CN103385837B CN 103385837 B CN103385837 B CN 103385837B CN 201310332090 A CN201310332090 A CN 201310332090A CN 103385837 B CN103385837 B CN 103385837B
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- myricae rubrae
- proanthocyanidin
- folium myricae
- astringent
- rubrae proanthocyanidin
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- Cosmetics (AREA)
Abstract
The invention discloses myrica rubra leaf proanthocyanidin toning lotion and a preparation method of the myrica rubra leaf proanthocyanidin toning lotion. According to 1L in volume, the myrica rubra leaf proanthocyanidin toning lotion comprises the following components: 50-200ml of ethanol, 50-150ml of glycerol, 1-20g of boracic acid, 0.2-1g of ascorbic acid, 0-0.5g of potassium hydroxide, 0.1-1g of myrica rubra leaf proanthocyanidin, 1-5g of Tween-20, a suitable amount of a preservative and a suitable amount of essence. According to the myrica rubra leaf proanthocyanidin toning lotion and the preparation method, the myrica rubra leaf proanthocyanidin toning lotion is prepared by taking the myrica rubra leaf proanthocyanidin extracted from myrica rubra leaves as a main functional component and being supplemented with by a suitable solvent, a suitable moisturizing agent, an suitable astringent, an suitable antioxidant and the like through appropriate ratios, and the obtained myrica rubra leaf proanthocyanidin toning lotion has the efficacies of resisting oxidation and aging, whitening, moisturizing and the like, and the stability of active ingredients is good, so that the myrica rubra leaf proanthocyanidin toning lotion is natural and safe.
Description
Technical field
The present invention designs cosmetic field, particularly relates to a kind of Folium Myricae rubrae proanthocyanidin astringent and preparation method thereof.
Background technology
Along with the develop rapidly of national economy, improving constantly of living standard, cosmetics have become necessary indispensable in people's daily life, the consumption demand of people to cosmetics is all increasing rapidly in many-sides such as quantity, kind or quality, and consumer starts to pursue more healthy, safe and effective cosmetics.Therefore, plant functional additive because of its action temperature and and multiple-effect, Cosmetic Market occupies more and more consequence.In recent years, whole world Ge great cosmetics company is all at emphasis research and development natural material/Organic Ingredients, for preparing cosmetics active component (Song Liya, He Congfen. the research and development [M] of cosmetics plant functional additive. Beijing: China Light Industry Press, 2011:21-24.).The patent of invention of notification number CN100420433C discloses a kind of pure natural plant additive of sun-proof cosmetic skin care product, mainly the ethanol extract of Flos Sophorae, Semen Ziziphi Spinosae, Radix Polygalae, Aloe, Fructus Myricae rubrae, Rhizoma Phragmitis, Flos Matricariae chamomillae, Fructus rhamni (Rhamnus davurica Pall.), Cortex Fraxini, Herba Menthae, Radix Glycyrrhizae prepares, for antitan agent, but the method floristics used is more, Waxberry fruit is one wherein, the anti-oxidation efficacy of product is not given prominence to, and is applied in cosmetics and also needs to study related process further.
Proanthocyanidin has very strong non-oxidizability, in beauty treatment with skin care, have the effect quite attracted eyeball especially.Domestic and international research shows, proanthocyanidin can resist the absorption of free radical, aging resistance, help vitamin C and E, reduce uv damage, reduce melanin deposition, the destruction of prevention collagen fiber and elastic fiber, skin is made to keep due elasticity, avoid wrinkle produce (Wei Shaomin. elastin degradation and skin aging and skin care item thereof are developed [J]. daily chemical industry, 1997,5:245-256.), the good reputation of " skin vitamin ", " oral cosmetic product " is even enjoyed in countries such as America and Europes.
Proanthocyanidin belongs to plant source flavonoid, is extensively to be present in one of botanic polyphenols.The plant proanthocyanidin of current research is maximum with procyanidin class, and typical example is as grape pip procyanidin.Fructus Myricae rubrae is the local product fruits of south China, at present about the research and utilization of Fructus Myricae rubrae is mainly based on Waxberry fruit.Cortex Myricae Rubrae (Cortex Myricae Esculentae) is evergreen all the year round, flourishing, has every year and is often taken as garbage by the Folium Myricae rubrae pruned in a large number and abandons.Having there are some researches show in Folium Myricae rubrae and be rich in aldehydes matter to have the biological activity such as antioxidation, anti-bacteria and anti-virus, is a kind of plant resources with potentiality to be exploited.
At present, existing research adopts discarded Folium Myricae rubrae to be that Folium Myricae rubrae proanthocyanidin prepared by raw material, but the functional product that Vehicles Collected from Market is developed for functional factor with Folium Myricae rubrae proanthocyanidin is also considerably less.Therefore, in view of the functional characteristic of Folium Myricae rubrae proanthocyanidin, developed as the cosmetic functional factor, for the production of there is antiinflammatory, UV resistance irradiation, skin care, removing the high effect cosmetic of the function such as speckle and whitening, have certain market prospect (Zhang Changgui, Dong Jiabao, Wang Zhenxu. proanthocyanidin and Application and Development [J] thereof. Sichuan food and fermentation, 2006,42 (1): 8-12.).
Summary of the invention
The invention provides a kind of Folium Myricae rubrae proanthocyanidin astringent, with Folium Myricae rubrae proanthocyanidin for functional active components, there is the effects such as antioxidation, defying age, whitening skin and preserving moisture, active component good stability, the natural safety of product.
A kind of Folium Myricae rubrae proanthocyanidin astringent, take water as substrate, in volume 1L, described Folium Myricae rubrae proanthocyanidin astringent comprises: ethanol 50-200mL, glycerol 50-150mL, boric acid 1-20g, ascorbic acid 0.2-1g, potassium hydroxide 0-0.5g, Folium Myricae rubrae proanthocyanidin 0.1-1g, tween 20 1-5g, Preservative qs, essence are appropriate.
Proanthocyanidin material has unique chemistry and physiologically active, multiple action is played in skin care item, as defying age, uvioresistant, radioprotective, brighten, moisturizing etc., unique effect (section Yuqin is had to the skin aging that many factors causes, Xie Bijun. procyanidin is in the research and development present situation [J] of cosmetic field. fragrance flavor and cosmetic, 2002,6:23-26).Folium Myricae rubrae proanthocyanidin can extract and obtain from Folium Myricae rubrae, there is good antioxidation, white-skinned face function, with it for functional components, then coordinate suitable solvent, wetting agent etc., can obtain and there is antiinflammatory, UV resistance irradiation, skin care, remove the astringent of speckle and white-skinned face function.
Preferably, in volume 1L, described Folium Myricae rubrae proanthocyanidin astringent comprises: ethanol 80-150mL, glycerol 80-120mL, boric acid 1-15g, ascorbic acid 0.2-0.8g, potassium hydroxide 0.1-0.2g, Folium Myricae rubrae proanthocyanidin 0.1-0.2g, tween 20 2-4g, Preservative qs, essence are appropriate.
Described Folium Myricae rubrae proanthocyanidin can be prepared by the following method:
(1) Folium Myricae rubrae powder is added in solvent carry out lixiviate, be separated and obtain extract;
(2) by column chromatography, separation and purification is carried out to extract, obtain Folium Myricae rubrae proanthocyanidin.
In step (1), described solvent can be aqueous acetone solution; The concentration of volume percent of aqueous acetone solution is preferably 60-80%, is more preferably 70%, and the aqueous acetone solution of this concentration range is conducive to the leaching of Folium Myricae rubrae Procyanidins material most.
Described Folium Myricae rubrae powder and the weight ratio of aqueous acetone solution are preferably 1:6-1:10, are more preferably 1:8.
In order to slow down the oxidation deterioration of leaching process Procyanidins, improving extracting effect, preferably, in described aqueous acetone solution, being added with the ascorbic acid that mass percent concentration is 0.01-1%.
Described extraction temperature is 15-35 DEG C, and extraction time is 4-12h, and under this condition, extracting effect is best.
In step (2), described column chromatography is gel permeation chromatography, and eluant used is aqueous acetone solution or methanol aqueous solution; Preferably, the aqueous acetone solution of described eluant to be concentration of volume percent be 45-55%, adopt this eluant, the fraction Procyanidins content of eluting gained can arrive 50-60%.
Folium Myricae rubrae proanthocyanidin adds as functional raw material, and its consumption is preferably 0.1-0.2g in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 0.12g, i.e. 0.12g/L.Show according to the result of study of Folium Myricae rubrae proanthocyanidin about non-oxidizability and tryrosinase inhibition, Folium Myricae rubrae proanthocyanidin has the activity removing ABTS, DPPH and ORAC free radical, iron ion reducing power is even far away higher than VC and myricetin, and it has suitable antioxidant activity as seen.In addition, when proanthocyanidin concentration reaches 0.06mg/mL, the tyrosinase inhibition rate of Folium Myricae rubrae proanthocyanidin reaches 51.23%, can 60.17% be reached when concentration is 0.12mg/mL, and be not difficult to find, from 0.06mg/mL, the trend that tyrosinase inhibition rate raises with concentration and improves slows down to some extent, when concentration reaches 0.12mg/mL, this kind of trend is more obvious.These factors relevant to beauty functions comprehensive, and each side's factor such as extraction process, yield, cost of consideration Folium Myricae rubrae proanthocyanidin, when the addition determining Folium Myricae rubrae proanthocyanidin is 0.12g/L, effect is better.
Owing to the addition of this natural function raw material of Folium Myricae rubrae proanthocyanidin in astringent of the present invention, therefore, astringent should be based upon give full play to this function raw material effect basis on, cosmetic base selected by all the other needs the stability farthest maintaining or improve Folium Myricae rubrae proanthocyanidin, and highlight its effect, play respective auxiliary effect, to reach optimum efficiency simultaneously.
Described ethanol except as except solvent, also has certain antibacterial, sterilization and antisepsis; In addition, ethanol has refrigerant effect, and can solidifying protein, reaches the object of tightening up skin; But meanwhile, the stimulation of ethanol can produce certain injury to skin, so will consumption be controlled, too much unsuitable.Consider, the consumption of ethanol is preferably 80-150mL in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 100mL, use the ethanol of 10% as mixed with water again after organic solvent dissolution fraction matrix, effect is better.
Described glycerol (glycerol) is clear and bright, colourless, odorless, thick liquid, and its moisture-keeping function is not easily oxidized under general holding conditions, more stable with the blend chemistry of water, ethanol, and can be used as the solvent of boric acid etc.Glycerol is added in astringent, can give the moisture that skin is suitable, with anti-drying, contribute to skin fitness.In addition, according to results of stability display, the stability of glycerol on Folium Myricae rubrae proanthocyanidin does not almost affect, another kind of wetting agent hyaluronate sodium then can along with the stability of the rising destruction proanthocyanidin of concentration, therefore, select glycerol to add as wetting agent, give up hyaluronate sodium.The consumption of glycerol is preferably 80-120mL in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 100mL.
Described boric acid, can balance skin pH value mainly as astringent, and conditioning fat secretion, plays Controlling oil effect.In addition, in order to alleviate the stimulation of astringent to skin, often non-ionic surface active agent is added.According to the result of stability study, boric acid may affect proanthocyanidin in the mode affecting pH, the pH scope of safety is 4.3 ~ 8.0, the boric acid pH of concentration within 2% is all not less than 4.3, but ascorbic acid and Folium Myricae rubrae proanthocyanidin itself all have certain acidity, so a certain amount of potassium hydroxide need be added to regulate pH.The consumption of boric acid is preferably 1-15g in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 10g, can good acid or alkali environment be maintained.
Described ascorbic acid (VC) is powerful antioxidant, and its aqueous solution is faintly acid, and stable in acidity, typical concentrations is 0.02-0.5%.According to results of stability, VC effectively can improve the stability of Folium Myricae rubrae proanthocyanidin.In addition, the reproducibility that VC has and check melanin make himself also to have certain white-skinned face function, better with Folium Myricae rubrae proanthocyanidin compatibility result of use.The consumption of ascorbic acid is preferably 0.2-0.8g in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 0.4g, effectively can strengthen the stability of Folium Myricae rubrae proanthocyanidin.
Described potassium hydroxide is mainly used in regulating pH, so that Folium Myricae rubrae proanthocyanidin maintains good stability.The consumption of potassium hydroxide will match with the consumption of boric acid, ascorbic acid, is preferably 0.1-0.2g in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 0.14g.
Described tween 20 is pale yellow oily liquid body, and water-soluble, ethanol, diluted acid etc., have the effect of cosolvent, stabilizing agent, play the effect of surfactant, compares other surfactant better effects if such as dodecyl sodium sulfate, fatty acid Pyrusussuriensis be smooth.But because tween 20 has fat smelly, when therefore using, to consumption be noted.The consumption of tween 20 is preferably 2-4g in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 3g.
Described antiseptic can be at least one in methyl hydroxybenzoate, potassium sorbate and sodium benzoate; Be preferably methyl hydroxybenzoate.Methyl hydroxybenzoate is a kind of antibiotic antiseptic, all effective in very wide pH scope (3 ~ 8), and has broad spectrum antibacterial, to yeast and mycete effect best; And, owing to having phenolic hydroxyl structure, so antibacterium Performance Ratio benzoic acid, sorbic acid are all strong; It is slightly soluble in water, is soluble in ethanol, has stimulation to skin, and China's " cosmetics health specification " (2007 editions) regulation, the limitation of single ester is 0.4%.According to stability study, methyl hydroxybenzoate on the stability of Folium Myricae rubrae proanthocyanidin almost without impact.The consumption of methyl hydroxybenzoate is preferably 0-0.4g in 1L Folium Myricae rubrae proanthocyanidin astringent; Be more preferably 0.4g.
Described essence can be at least one in Green tea essence, rose essence and Fructus Myricae rubrae essence; Be preferably the mixture of Green tea essence, rose essence, Fructus Myricae rubrae essence.Three kinds of essence, by the allotment of certain ratio, make astringent have pleasant abnormal smells from the patient; In addition, add Fructus Myricae rubrae essence and astringent can also be made to have characteristic odor, with add functional raw material---Folium Myricae rubrae proanthocyanidin matches.Preferably, the consumption of essence counts Green tea essence 0.5-1mL, rose essence 0.1-0.5mL with 1L Folium Myricae rubrae proanthocyanidin astringent, Fructus Myricae rubrae essence 0.01-0.1mL; Be more preferably Green tea essence 0.75mL, rose essence 0.2mL, Fructus Myricae rubrae essence 0.05mL.
Keep activity stabilized to make Folium Myricae rubrae proanthocyanidin, make each auxiliary element reach best of breed effect simultaneously, most preferably, in volume 1L, described Folium Myricae rubrae proanthocyanidin astringent comprises: ethanol 100mL, glycerol 100mL, boric acid 10g, ascorbic acid 0.4g, potassium hydroxide 0.14g, Folium Myricae rubrae proanthocyanidin 0.12g, tween 20 3g, methyl hydroxybenzoate 0.4g, Green tea essence 0.75mL, rose essence 0.2mL, Fructus Myricae rubrae essence 0.05mL.
Present invention also offers the preparation method of above-mentioned Folium Myricae rubrae proanthocyanidin astringent, comprising:
(1) glycerol is dissolved in part water, obtains glycerine water solution; Boric acid, ascorbic acid, potassium hydroxide are dissolved in remaining water, then add glycerine water solution, mixing, obtained aqueous phase;
(2) Folium Myricae rubrae proanthocyanidin is dissolved in a small amount of ethanol, obtains Folium Myricae rubrae proanthocyanidin solution; Antiseptic, tween 20, essence are dissolved in remaining ethanol successively, then add Folium Myricae rubrae proanthocyanidin solution, mixing, obtained alcohol phase;
(3) aqueous phase is mixed homogeneously mutually with alcohol, filter, leave standstill, obtained Folium Myricae rubrae proanthocyanidin astringent.
In step (1), because the object of adding potassium hydroxide regulates pH, in formula, major effect pH's has ascorbic acid and boric acid, therefore, first this three is mixed, and can reduce the impact of pH on Folium Myricae rubrae proanthocyanidin.
In step (2), the mass percent concentration of described ethanol can be 90%.Folium Myricae rubrae proanthocyanidin is first used the ethanol predissolve of 90%, not only contribute to the dissolving of proanthocyanidin, also contribute to the stable homogeneous of mixed liquor.
In step (3), after filtration, due to the existence of surface active agent tween-20, solution surface has more white foam, and by leaving standstill, foam can effectively cancellation.
The pH being prepared the astringent obtained by said method is 5.61, and the astringent pH=4.0 ~ 8.5(specified at QB/T2660-2004 directly surveys method) in scope (QB/T2660-2004. People's Republic of China (PRC) light industry standard (astringent) [S] .).And, this pH is also 5.22 ~ 7.55 within the scope of this, and under this environment, Folium Myricae rubrae proanthocyanidin is relatively more stable, and weakly acidic environmental benefits is in the stable (Wang Shujun of VC, distribution. cosmetics galenic pharmacy [M]. Shenyang: Liaoning science tech publishing house, 2012.).In addition, because the skin surface pH value of people is about 5.0 ~ 7.0, in faintly acid, so the astringent within the scope of this is relatively gentle, stimulate less.
The present invention, to obtain through refining the Folium Myricae rubrae proanthocyanidin that obtains in Folium Myricae rubrae for main composition, is aided with suitable solvent, surfactant, wetting agent, astringent, antioxidant etc., by suitable proportioning, prepares Folium Myricae rubrae proanthocyanidin astringent.
Adopt the inventive method, there is following beneficial effect:
(1) the astringent production liquid obtained by is even, and free from foreign meter, in emulsion form, fragrance pleasant, has light Fructus Myricae rubrae characteristic perfume.Astringent with Folium Myricae rubrae proanthocyanidin for natural function raw material, there is antioxidation, defying age, Bearberry Extract that proanthocyanidin has, and other compositions added are very little to Folium Myricae rubrae proanthocyanidin stability influence, effect of Folium Myricae rubrae proanthocyanidin at utmost can be played.In addition, owing to the addition of antioxidant VC and astringent boric acid, not only further enhance the anti-oxidation efficacy of astringent, also make it have certain convergence, effectively can nurse one's health fat secretion, play Controlling oil effect.
(2) astringent preparing process is simple, and drop into without the need to large number quipments, in equipment and technology, cost is lower.In addition, although market has various brand, the astringent of different efficacies is constantly developed out, but these astringent are mostly expensive, result of use is general, What is more exists more side effect, is not suitable for life-time service, astringent of the present invention due to add function raw material be plant extract, make it have less side effect, more natural full effect.
Accompanying drawing explanation
Fig. 1 is the antioxidation of Folium Myricae rubrae proanthocyanidin in the embodiment of the present invention 2, white-skinned face function and stability test result; Wherein, a is pH value impact effect figure, b be boric acid impact effect figure, c be glycerol impact effect figure, d be hyaluronate sodium impact effect figure, e be methyl hydroxybenzoate impact effect figure, f is VC impact effect figure.
Detailed description of the invention
The preparation of embodiment 1 Folium Myricae rubrae proanthocyanidin
(1) Folium Myricae rubrae is cleaned, remove disease and pest blade, pulverize after 40 DEG C of vacuum dryings, cross 40 mesh sieves.
(2) get 4kg Folium Myricae rubrae powder, be placed in 32L70%(v/v) aqueous acetone solution (being added with the ascorbic acid that mass percent concentration is 0.5%), lixiviate 4h under room temperature (25 DEG C), lixiviate three times; Collect merging three lixiviating solution, 40 DEG C of rotary evaporation removing acetone, filtered while hot, obtains about 30L aqueous solution and lyophilization, obtains about 400g extract, i.e. Folium Myricae rubrae proanthocyanidin crude extract EPAs.
(3) get 5g extract, be dissolved in methanol-water (1:1, v/v), be splined on Sephadex LH-20 chromatographic column (300 × 25mm).Adopt 50% methanol and 90% methanol aqueous solution as eluant successively, remove saccharide, pigment and most of flavone; Again with 50% aqueous acetone solution eluting, collect fraction, obtain Folium Myricae rubrae proanthocyanidin.
The antioxidation of embodiment 2 Folium Myricae rubrae proanthocyanidin, white-skinned face function and stability test
1, Folium Myricae rubrae proanthocyanidin, VC compare with the antioxidant activity of myricetin
Measure PA(Folium Myricae rubrae proanthocyanidin respectively by four kinds of modes), VC and Myr(myricetin) antioxidant activity, the results are shown in Table 1, as seen from table, Folium Myricae rubrae proanthocyanidin is close with VC in removing ABTS free radical, VC is weaker than in removing DPPH, ORAC free radical, but be the strongest in three to iron ion reducing power (FRAP method), show that Folium Myricae rubrae proanthocyanidin has good antioxidant activity.
The antioxidant activity of table 1 three kinds of materials compares
a(n=5)
a: represent that there were significant differences each other (p < 0.05) with the medium and small female difference of writing of string; Represent that there were significant differences each other (p < 0.05) with capitalization difference in a line.
2, Folium Myricae rubrae proanthocyanidin, VC compare with the tyrosinase inhibition rate of myricetin
As shown in Table 2, when concentration is 0.148mg/ml, the tyrosinase inhibition rate of PA reaches 61.3%, is only second to 76.1% of VC, and Myr only 32.6%; The tyrosinase inhibition rate of VC and PA all raises with the rising of concentration; When concentration is 0.02mg/ml ~ 0.06mg/ml, the tyrosinase inhibition rate of PA is the highest in three, but after concentration is greater than 0.06mg/ml, the trend that its suppression ratio raises with the rising of concentration slows down to some extent, after concentration reaches 0.12mg/ml, this sluggish trend is more obvious.Visible, consider production cost etc., PA is higher to tyrosinase inhibition rate when concentration 0.12mg/ml, and now whitening effect is better.
The tyrosinase inhibition rate (%) of table 2PA, VC and Myr compares
a(n=3)
a: letter is different represents that there were significant differences each other (p < 0.05).
3, pH is on the impact of Folium Myricae rubrae proanthocyanidin stability
Fig. 1 (a), for pH value is on the impact of Folium Myricae rubrae proanthocyanidin stability, as seen from the figure, when pH is in 5.22 ~ 7.55 scopes, affects without significance Folium Myricae rubrae proanthocyanidin.The pH of Folium Myricae rubrae proanthocyanidin solution self is 6.18, in faintly acid.Along with the increase of acidity or alkalinity, proanthocyanidin content all has decline, when pH is particularly evident in the outer downward trend of 4.3 ~ 8.0 scopes.As can be seen here, Folium Myricae rubrae proanthocyanidin is more responsive to soda acid, close to safer in the scope near itself pH value, and peracid or cross the reduction that alkali all can cause proanthocyanidin content.
4, astringent is on the impact of Folium Myricae rubrae proanthocyanidin stability
Employing boric acid is astringent, and the impact on Folium Myricae rubrae proanthocyanidin stability under mensuration variable concentrations, the results are shown in by Fig. 1 (b).Known, affect without significance Folium Myricae rubrae proanthocyanidin during boric acid concentration < 1%, along with the increase of boric acid concentration, the content of proanthocyanidin declines to some extent.Infer that the impact of boric acid on proanthocyanidin is main relevant with pH.
5, wetting agent is on the impact of Folium Myricae rubrae proanthocyanidin stability
Adopt glycerol and hyaluronate sodium as wetting agent respectively, the impact on Folium Myricae rubrae proanthocyanidin stability under mensuration variable concentrations, the results are shown in Figure 1(c) and (d).As seen from the figure, two kinds of wetting agent impacts on Folium Myricae rubrae proanthocyanidin are different.From the results of view, hyaluronate sodium has significance to proanthocyanidin, and glycerol then affects without significance.Along with the increase of hyaluronic acid na concn, the content of proanthocyanidin declines to some extent.
6, antiseptic is on the impact of Folium Myricae rubrae proanthocyanidin stability
Adopt methyl hydroxybenzoate as antiseptic, the impact on Folium Myricae rubrae proanthocyanidin stability under mensuration variable concentrations, the results are shown in Figure 1(e).As seen from the figure, in the concentration range of Setup Experiments, namely during addition < 0.04%, methyl hydroxybenzoate affects without significance Folium Myricae rubrae proanthocyanidin.
7, antioxidant is on the impact of Folium Myricae rubrae proanthocyanidin stability
Adopt VC as antioxidant, after mensuration interpolation variable concentrations VC, the change of Folium Myricae rubrae proanthocyanidin stability, the results are shown in Figure 1(f).As seen from the figure, after an interpolation VC, proanthocyanidin content creates change at once, this may with VC add that to change pH environment relevant, but, find in experiment afterwards, the stability of Folium Myricae rubrae proanthocyanidin significantly improves, and the proanthocyanidin content after 15 days is far away higher than blank group.In whole experimentation, nearly all proanthocyanidin content that with the addition of the sample after VC is all on blank group.In the concentration of Setup Experiments, along with the increase of VC concentration, the stability of Folium Myricae rubrae proanthocyanidin strengthens, when VC concentration reaches 0.4mg/ml, proanthocyanidin content reaches maximum, even if increase the concentration of VC subsequently again, the content of sample Procyanidins declines on the contrary, and this Changing Pattern is identical with the result of study of Wu Chaoxia.The reason producing this phenomenon may be VC extremely unstable, easy oxidized rear generation H
2o
2, thus cause proanthocyanidin to be oxidized.As polyphenolic substance, containing multiple ortho positions phenolic hydroxyl group, very easily there is oxidation polymerization and decomposition reaction in proanthocyanidin.At VC in the impact of Folium Myricae rubrae proanthocyanidin stability, the existing impact brought owing to changing pH of possibility, the result that produces after also may being the interphase interaction of the molecule newly added and proanthocyanidin molecule (Wu Chaoxia. Proanthocyanidins from Grape Seeds separating-purifying, component are identified and antioxidation is studied [D]. Shenyang: Agricultural University Of Shenyang, 2005:57-66.).
To sum up, above result is analyzed known:
(1) Folium Myricae rubrae proanthocyanidin has good antioxidation and white-skinned face function;
(2) as astringent, during boric acid concentration < 1%, Folium Myricae rubrae proanthocyanidin is affected without significance, but along with the rising of concentration, proanthocyanidin stability declines to some extent, mainly may to affect pH relevant with boric acid;
(3) as wetting agent, glycerol is less than the stability influence of hyaluronate sodium to Folium Myricae rubrae proanthocyanidin;
(4) concentration is lower than in 0.04% scope, antiseptic methyl hydroxybenzoate on proanthocyanidin almost without impact;
(5) VC is good antioxidant, effectively can improve the stability of Folium Myricae rubrae proanthocyanidin.
The preparation of embodiment 3 Folium Myricae rubrae proanthocyanidin astringent
Preparation 500ml whitening lotion, formula is as shown in table 3.
Table 3 astringent formula
Concrete compound method is as follows:
(1) 400ml pure water is measured, 50ml ethanol, stand-by;
(2) get the pure water of about 50ml, dissolve boric acid, ascorbic acid and potassium hydroxide;
(3) measure 50ml glycerol, be dissolved in remaining 350ml pure water, obtain glycerine water solution, and the 50ml aqueous solution obtained with step (2) is even, obtained aqueous phase;
(4) get 9ml alcoholic solution, add 1ml pure water, dissolve Folium Myricae rubrae proanthocyanidin, obtain Folium Myricae rubrae proanthocyanidin solution;
(5) in remaining 41ml alcoholic solution, methyl hydroxybenzoate is added, tween 20 is added again after dissolving, finally add essence (Green tea essence, rose essence and Fructus Myricae rubrae essence) perfumery, and the Folium Myricae rubrae proanthocyanidin solution obtained with step (4) mixes, obtained alcohol phase;
(6) aqueous phase is mixed mutually with alcohol, ultrasonic vibration 15min, increase and dissolve, solution mix homogeneously;
(7) filter, except dust, insoluble matter, leave standstill;
(8) bottle, sealing is preserved.
Obtained astringent production liquid is even, and free from foreign meter, in emulsion form, fragrance pleasant, has light Fructus Myricae rubrae characteristic perfume.
Should be noted in process for preparation: Folium Myricae rubrae proanthocyanidin first with the ethanol predissolve that concentration is 90%, not only will contribute to the dissolving of proanthocyanidin, also contribute to the stable homogeneous of mixed liquor; The object of adding potassium hydroxide regulates pH, and in formula, major effect pH's has ascorbic acid and boric acid, so, first this three to be mixed, reduce pH to the impact of proanthocyanidin; After filtration, due to the existence of surface active agent tween-20, solution surface has more white foam, needs the standing long time just can cancellation voluntarily.
Claims (9)
1. a Folium Myricae rubrae proanthocyanidin astringent, take water as substrate, it is characterized in that, in volume 1L, described Folium Myricae rubrae proanthocyanidin astringent comprises: ethanol 50-200mL, glycerol 50-150mL, boric acid 1-20g, ascorbic acid 0.2-1g, potassium hydroxide 0-0.5g, Folium Myricae rubrae proanthocyanidin 0.1-1g, tween 20 1-5g, Preservative qs, essence are appropriate.
2. Folium Myricae rubrae proanthocyanidin astringent according to claim 1, it is characterized in that, in volume 1L, described Folium Myricae rubrae proanthocyanidin astringent comprises: ethanol 80-150mL, glycerol 80-120mL, boric acid 1-15g, ascorbic acid 0.2-0.8g, potassium hydroxide 0.1-0.2g, Folium Myricae rubrae proanthocyanidin 0.1-0.2g, tween 20 2-4g, Preservative qs, essence are appropriate.
3. Folium Myricae rubrae proanthocyanidin astringent according to claim 1, is characterized in that, described Folium Myricae rubrae proanthocyanidin is prepared by the following method:
(1) Folium Myricae rubrae powder is added in solvent carry out lixiviate, be separated and obtain extract;
(2) by column chromatography, separation and purification is carried out to extract, obtain Folium Myricae rubrae proanthocyanidin.
4. Folium Myricae rubrae proanthocyanidin astringent according to claim 3, is characterized in that, in step (1), described solvent is aqueous acetone solution, and the weight ratio of Folium Myricae rubrae powder and aqueous acetone solution is 1:6-1:10.
5. Folium Myricae rubrae proanthocyanidin astringent according to claim 3, is characterized in that, in step (1), described extraction temperature is 15-35 DEG C, and extraction time is 4-12h.
6. Folium Myricae rubrae proanthocyanidin astringent according to claim 3, is characterized in that, in step (2), described column chromatography is gel permeation chromatography, and eluant used is aqueous acetone solution or methanol aqueous solution.
7. Folium Myricae rubrae proanthocyanidin astringent according to claim 1, is characterized in that, described antiseptic is at least one in methyl hydroxybenzoate, potassium sorbate and sodium benzoate.
8. Folium Myricae rubrae proanthocyanidin astringent according to claim 1, is characterized in that, described essence is at least one in Green tea essence, rose essence and Fructus Myricae rubrae essence.
9. the preparation method of Folium Myricae rubrae proanthocyanidin astringent as claimed in claim 1, is characterized in that, comprising:
(1) glycerol is dissolved in part water, obtains glycerine water solution; Boric acid, ascorbic acid, potassium hydroxide are dissolved in remaining water, then add glycerine water solution, mixing, obtained aqueous phase;
(2) Folium Myricae rubrae proanthocyanidin is dissolved in a small amount of ethanol, obtains Folium Myricae rubrae proanthocyanidin solution; Antiseptic, tween 20, essence are dissolved in remaining ethanol successively, then add Folium Myricae rubrae proanthocyanidin solution, mixing, obtained alcohol phase;
(3) aqueous phase is mixed homogeneously mutually with alcohol, filter, leave standstill, obtained Folium Myricae rubrae proanthocyanidin astringent;
Wherein, in volume 1L, described Folium Myricae rubrae proanthocyanidin astringent comprises: ethanol 50-200mL, glycerol 50-150mL, boric acid 1-20g, ascorbic acid 0.2-1g, potassium hydroxide 0-0.5g, Folium Myricae rubrae proanthocyanidin 0.1-1g, tween 20 1-5g, Preservative qs, essence are appropriate.
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| CN105919875A (en) * | 2016-06-12 | 2016-09-07 | 马殿伟 | Traditional Chinese medicine composition containing myrica rubra and applied to whitening cosmetics |
| CN107951806A (en) * | 2017-12-19 | 2018-04-24 | 广东真丽斯化妆品有限公司 | A kind of gentle more effect aloe skin care item and its preparation process |
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