CN103385837A - 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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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, relates in particular to a kind of Folium Myricae rubrae proanthocyanidin astringent and preparation method thereof.
Background technology
Develop rapidly along with national economy, improving constantly of living standard, cosmetics have become necessary indispensable in people's daily life, people are to increase rapidly in many-sides such as quantity, kind or quality to the consumption demand of cosmetics, and consumer starts to pursue more healthy, safe and effective cosmetics.Therefore, the plant functional additive because of its action temperature and and multiple-effect, occupy more and more consequence on Cosmetic Market.In recent years, each large cosmetics company of the whole world is all at emphasis research and development natural material/Organic Ingredients, be used 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, the ethanol extract that is mainly 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, be used for antitan agent, but the method floristics used is more, Waxberry fruit is wherein a kind of just, the anti-oxidation efficacy of product is outstanding, and is applied in cosmetics and also needs further research related process.
Proanthocyanidin has very strong non-oxidizability, has especially the effect that quite attracts eyeball aspect beauty treatment and skin care.Research both at home and abroad shows, proanthocyanidin can be resisted 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, make skin keep due elasticity, avoid wrinkle produce (Wei Shaomin. elastin laminin degraded and skin aging and skin care item thereof are developed [J]. daily chemical industry, 1997,5:245-256.), even enjoy the good reputation of " skin vitamin ", " oral cosmetics " in countries such as America and Europes.
Proanthocyanidin belongs to the plant source flavonoid, is extensively to be present in one of botanic polyphenols.The plant proanthocyanidin of research is maximum with the procyanidin class at present, typical example such as grape pip procyanidin.Fructus Myricae rubrae is the special product fruit of south China, and the research and utilization of at present relevant Fructus Myricae rubrae is mainly take Waxberry fruit as main.Cortex Myricae Rubrae (Cortex Myricae Esculentae) is evergreen all the year round, and is flourishing, has every year the Folium Myricae rubrae of being pruned in a large number often be taken as garbage and abandon.Existing research shows in Folium Myricae rubrae is rich in aldehydes matter, has the biological activitys such as antioxidation, anti-bacteria and anti-virus, is a kind of plant resources with potentiality to be exploited.
At present, it is that raw material prepares the Folium Myricae rubrae proanthocyanidin that discarded Folium Myricae rubrae is adopted in existing research, but the functional product of developing take the Folium Myricae rubrae proanthocyanidin as functional factor on Vehicles Collected from Market is also considerably less.Therefore, functional characteristic in view of the Folium Myricae rubrae proanthocyanidin, it is developed as the cosmetics functional component, for the production of having antiinflammatory, anti-ultra-vioket radiation, skin care, removing the high effect cosmetic of the functions such as speckle and whitening, have certain market prospect (Zhang Changgui, Dong Jiabao, Wang Zhenxu. proanthocyanidin and Application and Development thereof [J]. the Sichuan food and fermentation, 2006,42 (1): 8-12.).
Summary of the invention
The invention provides a kind of Folium Myricae rubrae proanthocyanidin astringent,, take the Folium Myricae rubrae proanthocyanidin as functional active components, have 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, antiseptic is appropriate, essence is appropriate.
The proanthocyanidin material has unique chemistry and physiologically active, play multiple action in skin care item, as defying age, uvioresistant, radioprotective, brighten, moisturizing etc., the skin aging that many factors is caused has unique effect (section Yuqin, Xie Bijun. procyanidin is in the research and development present situation [J] of cosmetic field. fragrance flavor and cosmetic, 2002,6:23-26).The Folium Myricae rubrae proanthocyanidin can extract and obtain from Folium Myricae rubrae, have antioxidation, white-skinned face function preferably, take it as functional components, then coordinate suitable solvent, wetting agent etc., can make and have antiinflammatory, anti-ultra-vioket radiation, 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, antiseptic is appropriate, essence is appropriate.
Described Folium Myricae rubrae proanthocyanidin can prepare by the following method:
(1) the Folium Myricae rubrae powder is added in solvent and carries out lixiviate, separate and obtain extract;
(2) by column chromatography, extract is carried out separation and purification, obtain the 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%, and more preferably 70%, the aqueous acetone solution of this concentration range is conducive to the leaching of Folium Myricae rubrae Procyanidins material most.
The weight ratio of described Folium Myricae rubrae powder and aqueous acetone solution is preferably 1:6-1:10, more preferably 1:8.
In order to slow down the oxidation deterioration of leaching process Procyanidins, improve extracting effect, preferably, be added with the ascorbic acid that mass percent concentration is 0.01-1% in described aqueous acetone solution.
Described extraction temperature is 15-35 ℃, 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, described eluant is that concentration of volume percent is the aqueous acetone solution of 45-55%, adopts this eluant, and the fraction Procyanidins content of eluting gained can arrive 50-60%.
The 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; 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, the Folium Myricae rubrae proanthocyanidin has the activity of removing ABTS, DPPH and ORAC free radical, the iron ion reducing power is even far away higher than VC and myricetin, and as seen it has suitable antioxidant activity.In addition, when proanthocyanidin concentration reaches 0.06mg/mL, the tyrosinase inhibition rate of Folium Myricae rubrae proanthocyanidin has reached 51.23%, when being 0.12mg/mL, concentration can reach 60.17%, and be not difficult to find, from 0.06mg/mL, tyrosinase inhibition rate slows down to some extent with the trend that the concentration rising improves, when concentration reached 0.12mg/mL, this kind trend was more obvious.Comprehensive these factors relevant to beauty functions, and each side's factors such as the extraction process of consideration Folium Myricae rubrae proanthocyanidin, yield, cost, when the addition of determining the Folium Myricae rubrae proanthocyanidin is 0.12g/L, effect is better.
Owing to having added this natural function raw material of Folium Myricae rubrae proanthocyanidin in astringent of the present invention, therefore, astringent should be based upon on the basis of giving full play to this function raw material effect, the stability of Folium Myricae rubrae proanthocyanidin need to farthest be kept or improve to all the other selected cosmetic bases, and highlight its effect, bring into play simultaneously auxiliary effect separately, to reach optimum efficiency.
Described ethanol is except as solvent, also has certain antibiotic, sterilization and antisepsis; In addition, ethanol has refrigerant effect, and can solidifying protein, reaches the purpose of tightening up skin; But simultaneously, the stimulation of ethanol can produce certain injury to skin, thus to control consumption, too much unsuitable.Consider, the consumption of ethanol is preferably 80-150mL in 1L Folium Myricae rubrae proanthocyanidin astringent; 100mL more preferably, mixed with water again after using 10% ethanol as organic solvent dissolution part substrate, effect is better.
Described glycerol (glycerol) is clear and bright, colourless, odorless, thick liquid, and its moisture-keeping function is difficult for oxidized, more stable with the blend chemistry of water, ethanol, and can be used as the solvent of boric acid etc. under general holding conditions.Glycerol is added in astringent, can give skin suitable moisture,, with anti-drying, helps skin fitness.In addition, according to results of stability, show the stability almost not impact of glycerol on the Folium Myricae rubrae proanthocyanidin, another kind of wetting agent hyaluronate sodium can destroy along with the rising of concentration the stability of proanthocyanidin, 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; 100mL more preferably.
Described boric acid is mainly as astringent, can balance skin pH value, and the conditioning fat secretion, play the effect of control oil.In addition,, in order to alleviate the stimulation of astringent to skin, often add non-ionic surface active agent.Result according to stability study, boric acid may affect proanthocyanidin in the mode that affects pH, the pH scope of safety is 4.3～8.0, concentration all can be lower than 4.3 with interior boric acid pH 2%, but ascorbic acid and Folium Myricae rubrae proanthocyanidin itself all have certain acidity, so need to add a certain amount of potassium hydroxide, regulate pH.The consumption of boric acid is preferably 1-15g in 1L Folium Myricae rubrae proanthocyanidin astringent; More preferably 10g, can keep acid or alkali environment preferably.
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 as can be known, VC can effectively improve the stability of Folium Myricae rubrae proanthocyanidin.In addition, the reproducibility that VC has and check melanin make himself also has 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; 0.4g more preferably, can effectively strengthen the stability of Folium Myricae rubrae proanthocyanidin.
Described potassium hydroxide is mainly used in regulating pH, so that the Folium Myricae rubrae proanthocyanidin is kept stability preferably.The consumption of potassium hydroxide will match with the consumption of boric acid, ascorbic acid, in 1L Folium Myricae rubrae proanthocyanidin astringent, is preferably 0.1-0.2g; 0.14g more preferably.
Described tween 20 is the pale yellow oily liquid body, and water-soluble, ethanol, diluted acid etc., have the effect of cosolvent, stabilizing agent, plays 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, to note consumption while therefore using.The consumption of tween 20 is preferably 2-4g in 1L Folium Myricae rubrae proanthocyanidin astringent; 3g more preferably.
Described antiseptic can be in methyl hydroxybenzoate, potassium sorbate and sodium benzoate at least a; Be preferably methyl hydroxybenzoate.Methyl hydroxybenzoate is a kind of antibiotic antiseptic, and is all effective in very wide pH scope (3～8), and has broad spectrum antibacterial, best to yeast and mycete effect; And, owing to having phenolic hydroxyl structure, so the antibacterium performance is all stronger than benzoic acid, sorbic acid; It is slightly soluble in water, is soluble in ethanol, and skin is had stimulation, China's " cosmetics health standard " (2007 editions) regulation, and limiting the quantity of of single ester is 0.4%.According to stability study as can be known, 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; 0.4g more preferably.
Described essence can be in green tea essence, rose essence and Fructus Myricae rubrae essence at least a; Be preferably the mixture of green tea essence, rose essence, Fructus Myricae rubrae essence.Three kinds of essence, by certain ratio allotment, make astringent have pleasant abnormal smells from the patient; In addition, add Fructus Myricae rubrae essence and can also make astringent have characteristic odor, with add functional raw material---the Folium Myricae rubrae proanthocyanidin matches.Preferably, the consumption of essence is counted green tea essence 0.5-1mL with 1L Folium Myricae rubrae proanthocyanidin astringent, rose essence 0.1-0.5mL, Fructus Myricae rubrae essence 0.01-0.1mL; Green tea essence 0.75mL more preferably, rose essence 0.2mL, Fructus Myricae rubrae essence 0.05mL.
In order to make the Folium Myricae rubrae proanthocyanidin keep activity stabilized, make simultaneously each auxiliary element reach the best of breed effect, 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.
The present invention also provides 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, mix, make water;
(2) the 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, mix, make pure phase;
(3) water is mixed homogeneously mutually with pure, filter, standing, make Folium Myricae rubrae proanthocyanidin astringent.
In step (1), because the purpose of adding potassium hydroxide is to regulate 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 the Folium Myricae rubrae proanthocyanidin.
In step (2), the mass percent concentration of described ethanol can be 90%.The Folium Myricae rubrae proanthocyanidin is first used 90% ethanol predissolve, not only helped the dissolving of proanthocyanidin, also help the stable homogeneous of mixed liquor.
In step (3), after filtration, due to the existence of surfactant tween 20, solution surface has more white foam, by standing, and effectively cancellation of foam.
The pH for preparing the astringent that obtains by said method is 5.61, at the astringent pH=4.0～8.5(of QB/T2660-2004 regulation, directly surveys method) in scope (QB/T2660-2004. People's Republic of China (PRC) light industry standard (astringent) [S] .).And, this pH is also in 5.22～7.55 these scopes, and under this environment, the Folium Myricae rubrae proanthocyanidin is relatively more stable, and weakly acidic environment is conducive to the stable (Wang Shujun of VC, distribution. cosmetics galenic pharmacy [M]. Shenyang: Liaoning science tech publishing house, 2012.).In addition,, because people's skin surface pH value is about 5.0～7.0, be faintly acid,, so the astringent in this scope is relatively gentle, stimulate less.
The present invention, to obtain through refining the Folium Myricae rubrae proanthocyanidin that obtains in Folium Myricae rubrae as 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, have following beneficial effect:
(1) prepared astringent finished product uniform liquid, free from foreign meter, is emulsion form, and the fragrance pleasant has light Fructus Myricae rubrae characteristic perfume.Astringent is take the Folium Myricae rubrae proanthocyanidin as the natural function raw material, have antioxidation, defying age, Bearberry Extract that proanthocyanidin has, and other compositions that add are very little to Folium Myricae rubrae proanthocyanidin stability influence, can at utmost bring into play the effect of Folium Myricae rubrae proanthocyanidin.In addition,, owing to having added antioxidant VC and astringent boric acid, not only further strengthen the anti-oxidation efficacy of astringent, also made it have certain convergence, can effectively nurse one's health fat secretion, played the effect of control oil.
(2) the astringent preparing process is simple, need not large number quipments and drops into, and cost is lower aspect equipment and technology.In addition, although there is the astringent of various brands, different efficacies constantly to be developed out on market, 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, and astringent of the present invention is because the function raw material that adds is plant extract, make it have still less side effect, more natural full effect.
Description of drawings
Fig. 1 is antioxidation, white-skinned face function and the stability test result of Folium Myricae rubrae proanthocyanidin in the embodiment of the present invention 2; Wherein, a is pH value impact effect figure, and b is boric acid impact effect figure, and c is glycerol impact effect figure, and d is hyaluronate sodium impact effect figure, and e is methyl hydroxybenzoate impact effect figure, and f is VC impact effect figure.
The specific embodiment
The preparation of embodiment 1 Folium Myricae rubrae proanthocyanidin
(1) Folium Myricae rubrae is cleaned, removed the disease and pest blade, pulverize after 40 ℃ of vacuum dryings, cross 40 mesh sieves.
(2) get 4kg Folium Myricae rubrae powder, be placed in 32L70%(v/v) aqueous acetone solution (be added with mass percent concentration be 0.5% ascorbic acid), the lower lixiviate 4h of room temperature (25 ℃), lixiviate three times; Collect and merge three lixiviating solution, 40 ℃ of rotary evaporations are removed acetone, and filtered while hot obtains approximately 30L aqueous solution and lyophilization, obtains approximately 400g extract, i.e. Folium Myricae rubrae proanthocyanidin crude extract EPAs.
(3) get the 5g extract, be dissolved in methanol-water (1:1, v/v), be splined on Sephadex LH-20 chromatographic column (300 * 25mm).Adopt successively 50% methanol and 90% methanol aqueous solution as eluant, remove saccharide, pigment and most of flavone; , with 50% aqueous acetone solution eluting, collect fraction again, obtain the Folium Myricae rubrae proanthocyanidin.
Antioxidation, white-skinned face function and the stability test of embodiment 2 Folium Myricae rubrae proanthocyanidins
1, the antioxidant activity of Folium Myricae rubrae proanthocyanidin, VC and myricetin relatively
Measure respectively PA(Folium Myricae rubrae proanthocyanidin by four kinds of modes), VC and Myr(myricetin) antioxidant activity, the results are shown in Table 1, as seen from table, the Folium Myricae rubrae proanthocyanidin is approaching with VC aspect removing ABTS free radical, be weaker than VC aspect removing DPPH, ORAC free radical, but be the strongest in the three to iron ion reducing power (FRAP method), show that the Folium Myricae rubrae proanthocyanidin has antioxidant activity preferably.
The antioxidant activity of three kinds of materials of table 1 relatively
a(n=5)
a: represent that with the medium and small letter difference of writing of string there were significant differences each other (p＜0.05); There were significant differences each other (p＜0.05) with the different expressions of capitalization in delegation.
2, the tyrosinase inhibition rate of Folium Myricae rubrae proanthocyanidin, VC and myricetin relatively
As shown in Table 2, when concentration was 0.148mg/ml, the tyrosinase inhibition rate of PA reached 61.3%, was 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 the three, but concentration greater than 0.06mg/ml after, its suppression ratio slows down to some extent with the trend that the rising of concentration raises, after concentration reached 0.12mg/ml, this sluggish trend was more obvious.As seen, consider production cost etc., PA is higher to tyrosinase inhibition rate when concentration 0.12mg/ml, and this moment, whitening effect was better.
The tyrosinase inhibition rate (%) of table 2PA, VC and Myr relatively
a(n=3)
a: there were significant differences each other (p＜0.05) for the different expressions of letter.
3, the impact of pH on Folium Myricae rubrae proanthocyanidin stability
Fig. 1 (a) is the impact of pH value on Folium Myricae rubrae proanthocyanidin stability, as seen from the figure, when pH is in 5.22～7.55 scopes, the Folium Myricae rubrae proanthocyanidin is affected without significance.The pH of Folium Myricae rubrae proanthocyanidin solution self is 6.18, is faintly acid.Along with the increase of acidity or alkalinity, proanthocyanidin content all has decline, when pH particularly evident in 4.3～8.0 outer decline trend of scope.This shows, the Folium Myricae rubrae proanthocyanidin is more responsive to soda acid, and is safer near the scope near itself pH value, peracid or cross alkali and all can cause the reduction of proanthocyanidin content.
4, the impact of astringent on Folium Myricae rubrae proanthocyanidin stability
Employing boric acid is astringent,, on the impact of Folium Myricae rubrae proanthocyanidin stability, the results are shown in by Fig. 1 (b) under the mensuration variable concentrations.As can be known, during boric acid concentration＜1%, the Folium Myricae rubrae proanthocyanidin is affected without significance, along with the increase of boric acid concentration, the content of proanthocyanidin descends to some extent.Infer that boric acid is main relevant with pH on the impact of proanthocyanidin.
5, the impact of wetting agent on Folium Myricae rubrae proanthocyanidin stability
Adopt respectively glycerol and hyaluronate sodium as wetting agent,, on the impact of Folium Myricae rubrae proanthocyanidin stability, the results are shown in Figure 1(c under the mensuration variable concentrations) and (d).As seen from the figure, two kinds of wetting agents are different on the impact of Folium Myricae rubrae proanthocyanidin.From result, hyaluronate sodium has significance to proanthocyanidin, and glycerol affects without significance.Along with the increase of hyaluronic acid na concn, the content of proanthocyanidin descends to some extent.
6, the impact of antiseptic on Folium Myricae rubrae proanthocyanidin stability
Adopt methyl hydroxybenzoate as antiseptic,, on the impact of Folium Myricae rubrae proanthocyanidin stability, the results are shown in Figure 1(e under the mensuration variable concentrations).As seen from the figure, in the concentration range that experiment arranges, namely during addition＜0.04%, methyl hydroxybenzoate affects without significance the Folium Myricae rubrae proanthocyanidin.
7, the impact of antioxidant on Folium Myricae rubrae proanthocyanidin stability
Adopt VC as antioxidant, after mensuration interpolation variable concentrations VC, the variation 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 has produced variation at once, this may be with to have changed the pH environment adding of VC relevant, still, after experiment in find, the stability of Folium Myricae rubrae proanthocyanidin obviously improves, and the proanthocyanidin content after 15 days is far away higher than the blank group.In whole experimentation, nearly all proanthocyanidin content of the sample after VC that added is all on the blank group.In the concentration that experiment arranges, increase along with VC concentration, the stability of Folium Myricae rubrae proanthocyanidin strengthens, proanthocyanidin content reaches maximum when VC concentration reaches 0.4mg/ml, even increase again subsequently the concentration of VC, the content of sample Procyanidins descends on the contrary, and this Changing Pattern is identical with the result of study of Wu Chaoxia.The reason that produces this phenomenon may be that VC is extremely unstable, easily oxidized rear generation H
2O
2Thereby, cause the proanthocyanidin oxidation.Proanthocyanidin, as polyphenolic substance, contains a plurality of ortho positions phenolic hydroxyl group, and oxidation polymerization and decomposition reaction very easily occur.In the impact of VC on Folium Myricae rubrae proanthocyanidin stability, may be existing owing to having changed the impact that pH brings, may be also the result that produces after the molecule that newly adds and proanthocyanidin molecule interaction (Wu Chaoxia. Proanthocyanidins from Grape Seeds separating-purifying, component are identified and antioxidation research [D]. Shenyang: Agricultural University Of Shenyang, 2005:57-66.).
To sum up, analyze above result as can be known:
(1) the Folium Myricae rubrae proanthocyanidin has antioxidation and white-skinned face function preferably;
(2) as astringent, during boric acid concentration＜1%, the Folium Myricae rubrae proanthocyanidin is affected without significance, but along with the rising of concentration, proanthocyanidin stability descends to some extent, mainly may to affect pH relevant with boric acid;
(3) as wetting agent, glycerol is less to the stability influence of Folium Myricae rubrae proanthocyanidin than hyaluronate sodium;
(4) concentration is lower than in 0.04% scope, the antiseptic methyl hydroxybenzoate on proanthocyanidin almost without impact;
(5) VC is good antioxidant, can effectively improve the stability of Folium Myricae rubrae proanthocyanidin.
The preparation of embodiment 3 Folium Myricae rubrae proanthocyanidin astringent
Preparation 500ml whitening lotion, fill a prescription as shown in table 3.
Table 3 astringent formula
Concrete compound method is as follows:
(1) measure the 400ml pure water, 50ml ethanol, stand-by;
(2) get the pure water of 50ml left and right, 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 that obtains with step (2) is even, makes water;
(4) get the 9ml alcoholic solution, add the 1ml pure water, dissolve the Folium Myricae rubrae proanthocyanidin, obtain Folium Myricae rubrae proanthocyanidin solution;
(5) add methyl hydroxybenzoate in remaining 41ml alcoholic solution, add again tween 20 after dissolving, add finally essence (green tea essence, rose essence and Fructus Myricae rubrae essence) perfumery, and with the Folium Myricae rubrae proanthocyanidin solution that step (4) makes, mix, make pure phase;
(6) water is mixed mutually with alcohol, ultrasonic concussion 15min, increase and dissolve, the solution mix homogeneously;
(7) filter, except dust, insoluble matter, standing;
(8) bottling, sealing is preserved.
Prepared astringent finished product uniform liquid, free from foreign meter, be emulsion form, the fragrance pleasant, have light Fructus Myricae rubrae characteristic perfume.
Should be noted in process for preparation: the Folium Myricae rubrae proanthocyanidin will be first 90% ethanol predissolve with concentration, not only helps the dissolving of proanthocyanidin, also helps the stable homogeneous of mixed liquor; The purpose of adding potassium hydroxide is to regulate pH, and in formula, major effect pH's has ascorbic acid and boric acid, so, first this three is mixed, reduce the impact of pH on proanthocyanidin; After filtration, due to the existence of surfactant tween 20, solution surface has more white foam, needs the just cancellation voluntarily of standing long time.
Claims (9)
1. 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, antiseptic is appropriate, essence is 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, antiseptic is appropriate, essence is appropriate.
3. Folium Myricae rubrae proanthocyanidin astringent according to claim 1, is characterized in that, described Folium Myricae rubrae proanthocyanidin prepares by the following method:
(1) the Folium Myricae rubrae powder is added in solvent and carries out lixiviate, separate and obtain extract;
(2) by column chromatography, extract is carried out separation and purification, obtain the 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 ℃, 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 a 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 a 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, mix, make water;
(2) the 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, mix, make pure phase;
(3) water is mixed homogeneously mutually with pure, filter, standing, make 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, antiseptic is appropriate, essence is appropriate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789354A (en) * | 2015-03-30 | 2015-07-22 | 浙江大学 | Application of myrica rubra leaf proanthocyanidin to lipid antioxidation |
| 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 |
| CN109394609A (en) * | 2018-10-11 | 2019-03-01 | 浙江大学华南工业技术研究院 | A kind of Waxberry leaf extract and preparation method thereof and the application in cosmetics |
| CN110194756A (en) * | 2019-07-22 | 2019-09-03 | 刘文倩 | A method of preparing low polymerization degree procyanidine |
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| CN102617535A (en) * | 2012-02-24 | 2012-08-01 | 浙江大学 | Method for extracting prodelphinidins from myrica rubra leaves |
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| CN102617535A (en) * | 2012-02-24 | 2012-08-01 | 浙江大学 | Method for extracting prodelphinidins from myrica rubra leaves |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789354A (en) * | 2015-03-30 | 2015-07-22 | 浙江大学 | Application of myrica rubra leaf proanthocyanidin to lipid antioxidation |
| 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 |
| CN109394609A (en) * | 2018-10-11 | 2019-03-01 | 浙江大学华南工业技术研究院 | A kind of Waxberry leaf extract and preparation method thereof and the application in cosmetics |
| CN110194756A (en) * | 2019-07-22 | 2019-09-03 | 刘文倩 | A method of preparing low polymerization degree procyanidine |
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