CN101966139B - Apocynum venetum extract, preparation method thereof and application thereof to cosmetics - Google Patents

Apocynum venetum extract, preparation method thereof and application thereof to cosmetics Download PDF

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CN101966139B
CN101966139B CN201010519626.5A CN201010519626A CN101966139B CN 101966139 B CN101966139 B CN 101966139B CN 201010519626 A CN201010519626 A CN 201010519626A CN 101966139 B CN101966139 B CN 101966139B
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extract
apocyni veneti
cosmetics
herba apocyni
filtrate
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CN101966139A (en
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刘起棠
张卫明
马世宏
孙达峰
孟繁杰
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Altay Gaubau Tea Co ltd
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NANJING INSTITUTE FOR COMPREHENSIVE UTILIZATION OF WILD PLANT CHINA CO-OP
XINJIANG GAUBAO KENDER CO Ltd
GAUBAU GREEN INDUSTRY (SHENZHEN) Co Ltd
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Abstract

The invention belongs to the field of herbal cosmetic additives and discloses an apocynum venetum extract, a preparation method thereof and application thereof to cosmetics. The apocynum venetum extract is prepared by the following steps of: removing impurities from dogbane leaves and washing the dogbane leaves; performing continuous countercurrent extraction for 30 to 90 minutes at the temperature of between 45 and 70 DEG C and then filtering to obtain filtrate, wherein the weight ratio of the dogbane leaves based on the dried weight to water is 1:8 to 1:20; adding a chitosan flocculating agent into the filtrate, standing, performing centrifugation and removing precipitates to obtain the clear solution of an extract; performing vacuum concentration; washing macroporous resins on the concentrated solution with distilled water to colorless; performing elution with ethanol at the concentration of 20 to 85 percent; detecting the eluent and collecting active ingredients; and spray drying to obtain the apocynum venetum extract with the total flavonoid content of over 30 percent. The apocynum venetum extract can be applied to developing functional cosmetics with effects of skin peroxidation resistance, senility delay, whitening, radiation resistance, sun protection, inflammation resistance, allergic resistance, bacterial inhibition, moistening, moisture maintenance and the like.

Description

A kind of Herba Apocyni veneti extract and preparation method thereof and the application in cosmetics
Technical field
The invention belongs to natural plants cosmetics additive field, relate to a kind of Herba Apocyni veneti extract and preparation method thereof and the application in cosmetics.
Background technology
Cosmetics industry in people's life in occupation of considerable status, wherein the functional component cosmetics that come from plant because of its use safety, action temperature and, Be very effective and extremely consumers.A lot of medicinal plants is applied to functional cosmetics successively and produces, and creates good Social and economic benef@.Therefore, the active components of plants extract that prepared by application Chinese medicine theory and modern science and technology more and more comes into one's own in daily chemical industry.
The applicating history of natural plants in beauty and skin care is long, namely occurs as far back as Qin Han dynasty, very prevailing to the Tang Dynasty.The material such as flavone, organic acid, oils and fats, alkaloid, quintessence oil, phlegmatic temperament, protein, aminoacid, vitamins, mineral, trace element, phytohormone contained in plant all can on the generation different effect of human body skin and impact.As plant flavonoids as skin-protecting factor anti-skin peroxidating and slow down aging, whitening, radioprotective, sun-proof, antiinflammatory, antiallergic, antibacterial in there is obvious effect, polysaccharide has moisture-keeping function, aminoacid energy skin nutrition, reduce wrinkle, and protein is also benefited to enhancing skin elasticity.Along with the progress of science and technology, numerous active component also can be extracted and separate, and this is that such plant creates condition in the application of natural household chemicals field.
Herba Apocyni veneti, Apocynaceae Apocynum crop, formal name used at school Apocynum L., perennial wild draft bast fibre plant.Folium Apocyni Veneti contains the chemical analysis such as a large amount of flavone, triterpene, organic acid, aminoacid, polysaccharide, nontoxic due to it, has no side effect, is particularly suitable as the function ingredients of natural cosmetics.Still Herba Apocyni veneti extract is not used for the report of cream kind or washing class cosmetics at present.
Summary of the invention
The object of this invention is to provide a kind of Herba Apocyni veneti extract.
Another object of the present invention is to provide the preparation method of above-mentioned Herba Apocyni veneti extract.
A further object of the invention is to provide the application of above-mentioned Herba Apocyni veneti extract in cosmetics.
The object of the invention is to be realized by following technical proposal:
A kind of Herba Apocyni veneti extract, this extract is obtained by following method:
A. Folium Apocyni Veneti roguing, cleaning;
B. adopt Continuous Countercurrent Extraction, Folium Apocyni Veneti is in dry weight, and Folium Apocyni Veneti and water weight ratio are 1:8 ~ 1:20, Extracting temperature 45 ~ 70 DEG C, and extraction time is 30 ~ 90min, filters to get filtrate;
C. filtrate adds chitosan flocculant, leaves standstill 3 ~ 8h, centrifugal, removes precipitation, obtains extract clear liquid;
D. vacuum concentration, cocnentration factor is 3:1 ~ 8:1, v/v, macroporous resin on concentrated solution, is washed with distilled water to colourless, and with 20 ~ 85% ethanol elutions, eluent detects collects active component, and spraying dry, obtains the Herba Apocyni veneti extract that general flavone content is greater than 30wt%.
Described Herba Apocyni veneti extract, its Raw Folium Apocyni Veneti is the Folium Apocyni Veneti of fresh Folium Apocyni Veneti or drying.
Described Herba Apocyni veneti extract, wherein Folium Apocyni Veneti roguing, cleaning step, roguing can adopt vibration separation screen, and Folium Apocyni Veneti use water cleans, scavenging period 10 ~ 20min.
Described Herba Apocyni veneti extract, wherein the consumption of flocculating agent chitosan is 0.05 ~ 0.3% of filtrate weight.
Described Herba Apocyni veneti extract, wherein macroporous resin is D101 type, DM301 type or AB-8 type.
The preparation method of described Herba Apocyni veneti extract, the method comprises the following steps:
A. Folium Apocyni Veneti roguing, cleaning;
B. adopt Continuous Countercurrent Extraction, Folium Apocyni Veneti is in dry weight, and Folium Apocyni Veneti and water weight ratio are 1:8 ~ 1:20, Extracting temperature 45 ~ 70 DEG C, and extraction time is 30 ~ 90min, filters to get filtrate;
C. filtrate adds chitosan flocculant, leaves standstill 3 ~ 8h, centrifugal, removes precipitation, obtains extract clear liquid;
D. vacuum concentration, cocnentration factor is 3:1 ~ 8:1, v/v, macroporous resin on concentrated solution, is washed with distilled water to colourless, and with 20 ~ 85% ethanol elutions, eluent detects collects active component, and spraying dry, obtains general flavone content and be greater than 30% Herba Apocyni veneti extract.
The application of described Herba Apocyni veneti extract in cream kind cosmetics or washing class cosmetics.
Described application, wherein the addition of Herba Apocyni veneti extract in cream kind cosmetics is 0.3 ~ 5% by mass percentage.
Described application, wherein the addition of Herba Apocyni veneti extract in washing class cosmetics is 0.5 ~ 8% by mass percentage.
Advantage of the present invention:
(1) the natural green daily use chemicals raw material that is applied as of Herba Apocyni veneti extract provides more functional component to select;
(2) continuous countercurrent extraction process is owing to realizing continued operation, therefore can significantly improve production capacity in large-scale production, simultaneously to raising raw material availability, save cost and there is important realistic meaning the aspect such as to boost productivity.
(3) to have technique simple in the preparation of Herba Apocyni veneti extract, active component content is high, can standardized production and application, function is remarkable, may be used for developing the functionalization cosmetic of the effect such as anti-skin peroxidating and slow down aging, whitening, radioprotective, sun-proof, antiinflammatory, antiallergic, antibacterial, moist, moisturizing.
One, anti-oxidation function animal experiment report
(1) materials and methods
1, given the test agent: Herba Apocyni veneti extract, prepares by the embodiment of the present invention 1, lower same.
2, experimental animal: 12-14 monthly age SD male and healthy rat, western pul-Bi Kai laboratory animal company limited provides by Shanghai.
3, reagent: superoxide dismutase (SOD), lipid peroxide (MDA) builds up Bioengineering Research Institute by Nanjing provides.
4, dosage grouping: Herba Apocyni veneti extract human body recommended intake is 360mg/ people/day (by 60kg weighing machine), be equivalent to 6mg/kgbw, press respectively human body recommended intake 5 times, 10 times, 30 times designs low (30mg/kgbw), in (60mg/kgbw), high (180mg/kgbw) three dosage groups, separately establish matched group (0mg/kgbw), replace sample with sterilized water.Sample sterilized water is prepared, and basic, normal, high dose concentration is respectively 3mg/ml, 6mg/ml, 18mg/ml, and per os gives the tested material of rat respective concentration once a day, by 10ml/kgbw gavage, surveys every Antioxidant Indexes after continuous 21 days.
5, test method:
Rat buy after Animal House endoadaptation environment 5 days, get blood through eye socket, measure lipid peroxide (MDA) content in its serum.According to MDA content in rat blood serum, be divided into 4 groups at random, often organize 10, requirement of according to dosage dividing into groups is respectively blank group, basic, normal, high dosage group.Test group gives the Herba Apocyni veneti extract of corresponding dosage, and blank group replaces given the test agent with sterilized water, every day gavage, continuous 21 days.Content of MDA, SOD vigor is measured after 21 days.
6, rearing conditions: rat temperature be 18-25 DEG C, relative humidity is raise in the barrier system of 50-70%.
7, data analysis: carry out homogeneity test of variance to each experiment initial data with SPSS10.0 software, to meet in the data information one factor analysis of variance method that variance requires together the comparative approach between two of mean between multiple experimental group and a matched group and carries out statistical disposition; Suitable variable transitions is carried out to the data information of nonnormal distribution or heterogeneity of variance, after meeting normal distribution or variance and requiring together, carries out statistical disposition by the data of conversion gained.
(2) result:
1, Herba Apocyni veneti extract is on the impact of lipid peroxide in rat serum (MDA) content
From table 1, before experiment, in rat serum, MDA content compares with between matched group group in basic, normal, high three dosage groups, and there are no significant for difference (P>0.05).Namely before experiment, in rat serum, MDA content is comparatively balanced between respectively organizing.
Per os gives the Herba Apocyni veneti extract 21 days of rat various dose, MDA content in measured each dosage group rat serum is carried out homogeneity test of variance, meet homogeneity of variance requirement, statistical disposition is carried out with the comparative approach between two of mean between experimental group multiple in one factor analysis of variance method and a matched group, as shown in Table 2, after experiment, in basic, normal, high three dosage group rat serum, MDA content is compared with matched group, and there are no significant for difference (P>0.05).
Table 1: Herba Apocyni veneti extract on the impact of MDA content in rat serum (n=10, )
Group MDA (nmol/ml) before experiment P MDA (nmol/ml) after experiment P
Matched group 3.52±0.41 4.60±0.79
Low dose group 3.51±0.45 1.000 4.01±1.01 0.481
Middle dosage group 3.50±0.36 1.000 4.33±1.34 0.898
High dose group 3.49±0.51 0.996 3.55±0.92 0.085
2, Herba Apocyni veneti extract is on the impact of superoxide dismutase in rat serum (SOD) vigor
Per os gives the Herba Apocyni veneti extract 21 days of rat various dose, SOD vigor in measured each dosage group rat serum is carried out homogeneity test of variance, meet homogeneity of variance requirement, statistical disposition is carried out with the comparative approach between two of mean between experimental group multiple in one factor analysis of variance method and a matched group, as shown in Table 2, in basic, normal, high three dosage group rat serum, SOD vigor is significantly higher than matched group.
Table 2: Herba Apocyni veneti extract on the impact of SOD vigor in rat serum (n=10, )
Group SOD in serum (U/ml) P
Matched group 371±84
Low dose group 556±62 0.000
Middle dosage group 536±113 0.001
High dose group 589±102 0.000
Two. Herba Apocyni veneti extract anti-inflammation test: the inhibitory action test of mice caused by dimethylbenzene xylene ear swelling
Get kunming mice, by body weight random packet, continuous gastric infusion 6 days, fasting 12 hr overnight, is administered once on the 7th day again, and last administration is after 1 hour, and at two sides, the front and back even spread dimethylbenzene 0.05mL of mouse right ear, left ear is left intact.Put to death mice respectively at causing scorching latter 60 minutes de-cervical vertebras for each group, cut ears 7mm diameter card punch and lay round auricle in ears same area respectively, electronic balance claims quality.Calculate swelling and inhibitory rate of intumesce, compare administration group and matched group difference condition, between statistics employing group, t-student inspection, the results are shown in Table 3.Computing formula is:
Swelling (mg)=auris dextra tablet quality (mg)-left auricle quality (mg)
Inhibitory rate of intumesce=(matched group swelling-administration group swelling) ÷ matched group swelling × 100%.
Table 3. Herba Apocyni veneti extract xylol causes the inhibitory action result of the test of mice ear
Note: (1) .**:P<0.01, compares with matched group (t inspection)
(2) swelling (mg)=auris dextra sheet weight-left auricle weight
(3) inhibitory rate of intumesce (%)=(matched group swelling-administration group swelling)/matched group swelling * 100%
Result of the test shows, the auricle swelling degree of the high, medium and low dosage group of Herba Apocyni veneti extract compares with matched group pole significant difference (P<0.01), illustrates that Herba Apocyni veneti extract xylol causes mice ear and has extremely significant inhibitory action.And along with the increase of Herba Apocyni veneti extract dosage, inhibitory action increases, but amount-result relation between dosage and antiinflammatory action curative effect is not obvious.
Three, Antibacterial Activity
Adopt inhibition zone method, make plating medium, the bacterium liquid of quantitative debita spissitudo is coated with in the medium, take out the filter paper after dry heat sterilization, be placed in the Herba Apocyni veneti extract sample of variable concentrations respectively, after soaking 2min, put on the flat board containing bacterium according to the requirement of sterile working.Put into electronics biochemical cultivation case 37 DEG C cultivation.With vernier caliper measurement antibacterial circle diameter D (mm).Repeat for three times.
Experimental studies results shows (table 4): Herba Apocyni veneti extract has inhibitory action to pathogenic fungi, and inhibitory effect all presents certain dosage effect, and namely along with the increase of concentration, inhibitory action is more obvious.
Table 4 Herba Apocyni veneti extract is to staphylococcus aureus and streptococcic inhibitory action (X ± S, n=9)
Detailed description of the invention
The invention will be further elaborated by the following examples.
Embodiment 1
10 kilograms of Folium Apocyni Venetves (dry weight) roguing (can vibration separation screen be adopted), clean water 15min; Adopt Continuous Countercurrent Extraction, add water 160 kilograms, Extracting temperature 45 ~ 50 DEG C, being fed to discharging control extraction time is 60min, obtains filtrate by coarse filtration equipment; Filtrate adds chitosan flocculant 0.1 kilogram, leaves standstill 5h, and tube bank centrifuge high speed centrifugation, removes precipitation, obtain extract clear liquid 120 kg; Vacuum concentration, cocnentration factor is 6:1, v/v, D101 macroporous resin on concentrated solution, be washed with distilled water to colourless, use 75% ethanol elution, eluent detects collects active component, vacuum concentration, spraying dry, obtains Herba Apocyni veneti extract 1.2 kilograms, detects general flavone content 32.6wt%.
Embodiment 2
100 kilograms of Herba Apocyni veneti fresh leafs roguing (can vibration separation screen be adopted), clean water 15min; Adopt Continuous Countercurrent Extraction, add water 100 kilograms, Extracting temperature 55 ~ 60 DEG C, being fed to discharging control extraction time is 45min, obtains filtrate by coarse filtration equipment; Filtrate adds chitosan flocculant 0.2 kilogram, leaves standstill 8h, and tube bank centrifuge high speed centrifugation, removes precipitation, obtain extract clear liquid 150 kilograms; Vacuum concentration, cocnentration factor is 5:1, v/v, AB-8 macroporous resin on concentrated solution, be washed with distilled water to colourless, use 80% ethanol elution, eluent detects collects active component, vacuum concentration, spraying dry, obtains Herba Apocyni veneti extract 1.4 kilograms, detects general flavone content 35.2wt%.
Embodiment 3: the application of Herba Apocyni veneti extract in cream kind cosmetics
Moisturizer formula and processing technology:
A group is mixed, is heated to 75 DEG C; B group is mixed, is heated to 75 DEG C.Under agitation, A group is added on the emulsifying of B group, when temperature is down to 45 DEG C, adds essence.Through chemically examine qualified after, pack.
Embodiment 4: the application of Herba Apocyni veneti extract in washing class cosmetics
Shampoo formula and processing technology:
A, G is soluble in water, add B, C, E and F, heating for dissolving, then add D, H, use Fructus Citri Limoniae acid for adjusting pH, through chemically examine qualified after, pack.

Claims (4)

1. a Herba Apocyni veneti extract is preparing the application in cream kind cosmetics or washing class cosmetics; This extract is obtained by following method:
A. fresh or dry Folium Apocyni Veneti roguing, cleaning;
B. adopt Continuous Countercurrent Extraction, Folium Apocyni Veneti is in dry weight, and Folium Apocyni Veneti and water weight ratio are 1:8 ~ 1:20, Extracting temperature 45 ~ 70 DEG C, and extraction time is 30 ~ 90min, filters to get filtrate;
C. filtrate adds chitosan flocculant, and the consumption of flocculating agent chitosan is 0.05 ~ 0.3% of filtrate weight, leaves standstill 3 ~ 8h, centrifugal, removes precipitation, obtains extract clear liquid;
D. vacuum concentration, cocnentration factor is 3:1 ~ 8:1, v/v, macroporous resin on concentrated solution, is washed with distilled water to colourless, and with 20 ~ 85% ethanol elutions, eluent detects collects active component, and spraying dry, obtains general flavone content and be greater than 30% Herba Apocyni veneti extract.
2. application according to claim 1, is characterized in that macroporous resin is D101 type, DM301 type or AB-8 type.
3. application according to claim 1, is characterized in that the addition of Herba Apocyni veneti extract in cream kind cosmetics is 0.3 ~ 5% by mass percentage.
4. application according to claim 1, is characterized in that the addition of Herba Apocyni veneti extract in washing class cosmetics is 0.5 ~ 8% by mass percentage.
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CN102197887B (en) * 2011-05-23 2013-04-17 新疆戈宝红麻有限公司 Health-care brassiere made of Apocynum venetum Linn
CN103169632A (en) * 2011-12-22 2013-06-26 黄玉良 Application of dogbane leaf extract in preparation of skin-care product
CN105326716A (en) * 2015-11-30 2016-02-17 胡娟 Plant liquid shampoo or paste shampoo with hair washing and nourishing function and preparation method thereof
CN107365144A (en) * 2017-07-26 2017-11-21 广东康世泰新材料科技股份有限公司 A kind of ceramic of anti-Staphylococcus aureus and preparation method thereof
CN109223666B (en) * 2018-12-04 2021-05-25 施莱新研(杭州)生物科技有限公司 Plant extract composition and application thereof in skin care products
CN109276527B (en) * 2018-12-10 2021-05-21 北京市芳华世纪商贸有限公司 Plant extract and application thereof in cosmetics
CN110755277B (en) * 2019-12-05 2022-08-09 新疆维吾尔自治区中药民族药研究所 Toothpaste containing various plant extracts and preparation method thereof
CN110960457A (en) * 2019-12-11 2020-04-07 香港科技大学深圳研究院 Preparation method of apocynum venetum extract and application of apocynum venetum extract in whitening and skin-care products
WO2021160104A1 (en) * 2020-02-11 2021-08-19 厦门大学 Folium apocyni veneti extract, and preparation method therefor and use thereof
CN112494360A (en) * 2020-12-28 2021-03-16 中华全国供销合作总社南京野生植物综合利用研究所 Extraction method of apocynum venetum polysaccharide extract, apocynum venetum polysaccharide extract and application
CN112516014B (en) * 2021-01-08 2023-04-14 中华全国供销合作总社南京野生植物综合利用研究所 Apocynum venetum extract, preparation method thereof, anti-ultraviolet, anti-oxidation and whitening cosmetic and preparation method thereof
CN114533632A (en) * 2022-03-31 2022-05-27 陕西理工大学 Anti-aging moisturizing black wolfberry and apocynum venetum face cream and preparation method thereof

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