CN105078803A - Application of callicarpa plant extract - Google Patents
Application of callicarpa plant extract Download PDFInfo
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- CN105078803A CN105078803A CN201410208522.0A CN201410208522A CN105078803A CN 105078803 A CN105078803 A CN 105078803A CN 201410208522 A CN201410208522 A CN 201410208522A CN 105078803 A CN105078803 A CN 105078803A
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- callicarpae formosanae
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Abstract
The invention provides application of callicarpa plant extract in preparation of cosmetics used for removing freckles, whitening skin, removing wrinkles, protection from sun or preventing aging. The callicarpa plant extract has functions of suppressing activity of tyrosinase, clearing free radicals, reducing ultraviolet absorption and resisting skin aging. Callicarpa plants are extensive in source, long in using history and simple in extract preparation process. The callicarpa plant extract is a cosmetic functional raw material which is economically affordable, safe and effective. The invention further provides the cosmetics prepared by the callicarpa plant extract.
Description
Technical field
The present invention relates to cosmetic field, be specifically related to Callicarpa plant extract and preparing the purposes in cosmetics.
Background technology
Skin is the maximum organ-tissue of human body, and health can be prevented to be subject to the invasion of extraneous harmful factor (as ultraviolet, chemical irritant, heavy metal and some exogenous pollution things).Except the natural functions degeneration that the age brings, the factor such as the life style of modern fast pace, high pressure, immoderate diet, ecological deterioration accelerates degeneration and the aging of skin function, causes a series of skin problem.
Modern study thinks that human body can produce excessive reactive oxygen free radical in metabolic process, will produce oxidative damage, thus cause skin aging, degeneration, relaxes, follows the string, form wrinkle if removed not in time to skin.Therefore scavenging capacity oxygen-derived free radicals is exactly one of important means preventing and improve skin aging problem.For this reason, people use various antidotal cosmetics, mainly directly play antioxidation by adding antioxidant (as SOD, vitamin E etc.), this kind of cosmetics have certain anti-aging effects, but mostly can not effectively solve above-mentioned skin problem.
Folium Callicarpae Formosanae is the common name of Verenaceae (Verbenaceae) Callicarpa (CallicarpaL.) plant, of a great variety, about 190 kinds, and record according to " Chinese Plants will ", nearly 46 kinds of China, distributes comparatively extensive.Composition contained by Folium Callicarpae Formosanae is mainly flavonoid, terpenoid, phenethyl alcohol glycosides and volatile oil etc.Supplement to the Herbal that CHEN Zang-Qi is shown between the first year is opened first appeared in Tang, in history tree books, many places are recorded, there is the functions such as sterilization, antiinflammatory, hemostasis, as supplement to the Herbal is recorded: " separate all poisonous substances; carbuncle, sore throat, fly that corpse diseases due to noxious agents produced by various parasites, poison are swollen, lower fistula, Serpentis a poisonous snake mentioned in ancient books poison chela, mad dog poison; and liquor clothes; also liquor is washed skin ulcer and swollen, dehematize, longue ", Compendium of Material Medica is recorded: " promoting blood circulation and detumescence; diuresis and detoxifying; control all toxic swellings of all carbuncle carbuncle on the back multiple abscesss ", and " Fujian traditional herbal medicine " is recorded: " stasis of blood of living, hemostasis, antiinflammatory, resolving depression ".In recent years, about various effects of Folium Callicarpae Formosanae are reported, such as, Chinese patent application No.200810189027.4 discloses the beautyberry toothpaste with heat clearing and inflammation relieving, hemostasis, antibacterial, analgesic activity.Chinese patent application No.200910002488.0 discloses the purple beautyberry mouth wash with heat clearing and inflammation relieving, hemostasis, antibacterial, analgesic activity.Chinese patent application No.201110210953.7 discloses the application of a kind of Callicarpa nudiflora extract in daily use chemicals cleaning product.Chinese patent application No.200910036486.3 discloses the application of Callicarpa nudiflora extract in the oral-cavity cleaning products slowing down the various symptom of dental gingival hemorrhage, gingivitis and oral ulcer that people often suffer from.Have not yet to see the report of the application aspect of Callicarpa plant in speckle dispelling, whitening, wrinkle removal, sun-proof or anti-senescence function cosmetics.
Summary of the invention
Callicarpa plant extract is the object of the present invention is to provide to prepare the purposes in cosmetics.Described cosmetics have speckle dispelling, whitening, wrinkle removal, sun-proof or anti-ageing aging effect.
The invention provides following technical scheme:
1, Callicarpa plant extract is for the preparation of the purposes in speckle dispelling, whitening, wrinkle removal, sun-proof or anti-aging cosmetics.
2, the purposes according to technical scheme 1, wherein by weight, described cosmetics contain 0.1-10.0% Callicarpa plant extract, preferably contain the Callicarpa plant extract of 0.5 ~ 5.0%, are more preferably the Callicarpa plant extract of 1.0 ~ 3.0%.
3, the purposes according to technical scheme 1 or 2, wherein said Callicarpa plant extract is prepared by the stem of Verenaceae Callicarpa plant and/or leaf.
4, purposes according to any one of technical scheme 1-3, wherein said Verenaceae Callicarpa plant is selected from sharp leaf Folium Callicarpae Formosanae (CallicarpaacutifoliaH.T.Chang), different leaf Folium Callicarpae Formosanae (Callicarpaanisophylla), wood Folium Callicarpae Formosanae (CallicarpaarboreaRoxb.Hort.Beng), Folium Callicarpae Formosanae (CallicarpabodinieriLevl.), Callicarpa brevipes (Benth.) Hance (Callicarpabrevipes (Benth.) Hance), Folium Callicarpae candicantis (Callicarpacandicans (Burm.f.) Hochr.), callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang), Jinyun Folium Callicarpae Formosanae (CallicarpachinyunensisP ' eietW.Z.Fang), hills Folium Callicarpae Formosanae (CallicarpacollinaDiels), multiple tooth Folium Callicarpae Formosanae (Callicarpadentosa (H.T.Chang) W.Z.Fang), Callicarpa dichotoma (Callicarpadichotoma (Lour) K.Koch), red body Folium Callicarpae Formosanae (CallicarpaerythrostictaMerr.etChun), callicarpa pedunculata (CallicarpaformosanaRolfe), Radix Callicarpae Giraldii (CallicarpagiraldiiHesseexRehd), Hubei Folium Callicarpae Formosanae (CallicarpagracilipesRehd), thick calyx Folium Callicarpae Formosanae (CallicarpahungtaiiP ' eietS.L.Chen), entire beautyberry herb (CallicarpaintegerrimaChamp), Japan Folium Callicarpae Formosanae (CallicarpajaponicaThunb), callicarpa kochiana (CallicarpakochianaMakino), reddish tone Folium Callicarpae Formosanae (CallicarpakotoensisHayata), Callicarpa kwangtungensis Chun (CallicarpakwangtungensisChun), light leaf Folium Callicarpae Formosanae (CallicarpalingiiMerr), Callicarpa lobo-apiculata Metc. (CallicarpaloboapiculataMetc.), long luxuriant Folium Callicarpae Formosanae (CallicarpalongibracteataH.T.Chang), Folium Callicarpae Loureiri (CallicarpalongifoliaLamk.), long handle Folium Callicarpae Formosanae (CallicarpalongipesDunn), Folium Callicarpae Longissimae (Callicarpalongissima (Hemsl.) Merr.), yellow gland Folium Callicarpae Formosanae (CallicarpaluteopunctataH.T.Chang), Folium Callicarpae Macrophyllae (CallicarpamacrophyllaVahl), Callicarpa nudiflora (CallicarpanudifloraHook.), sieve floats Folium Callicarpae Formosanae (CallicarpaoliganthaMerr.), spend Folium Callicarpae Formosanae (CallicarpapaucifloraChunexH.T.Chang) less, glochild Folium Callicarpae Formosanae (CallicarpapeichienianaChunetS.L.Chen), rattan Folium Callicarpae Formosanae (CallicarpapeiiH.T.Chang), become mildewed Folium Callicarpae Formosanae (CallicarpapilosissimaMaxim.), Pingshan Folium Callicarpae Formosanae (CallicarpapingshanensisC.Y.WuexW.Z.Fang), white back of the body Folium Callicarpae Formosanae (CallicarpapoilaneiP.Dop), to sprout Folium Callicarpae Formosanae (CallicarpaproliferaC.Y.Wu), intend Folium Callicarpae Rubellae (CallicarpapseudorubellaH.T.Chang), the large Folium Callicarpae Formosanae of mountains in a range (CallicarparandaiensisHayata), dredge tooth Folium Callicarpae Formosanae (CallicarparemotiserrulataHayata), Folium Callicarpae Rubellae (CallicarparubellaLindl.), water JINHUA (CallicarpasalicifoliaP ' eietW.Z.Fang), upper lion Folium Callicarpae Formosanae (Callicarpasiong-saiensisMetc.), ancient cooking vessel lake Folium Callicarpae Formosanae (CallicarpatingwuensisH.T.Chaug) and Yunnan Folium Callicarpae Formosanae (CallicarpayunnanensisW.Z.Fang).
5, the purposes according to any one of technical scheme 1-4, wherein said Verenaceae Callicarpa plant is selected from callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang), callicarpa pedunculata (CallicarpaformosanaRolfe), Folium Callicarpae Macrophyllae (CallicarpamacrophyllaVahl) and Callicarpa kwangtungensis Chun (CallicarpakwangtungensisChun).
6, the purposes according to any one of technical scheme 1-5, wherein said Callicarpa plant extract is prepared by the method comprised the following steps:
(1) stem of Callicarpa plant and/or leaf (being preferably dry stem and/or leaf) are pulverized, with solvent extraction 1 ~ 3 time, described solvent is the mixture of water, ethanol or water and ethanol;
(2) each extracting solution is merged, the solvent described in concentrating under reduced pressure removing step (1); Add the water of 0.5 times ~ 2 times of volumes, hold over night, centrifugal or filtration obtains supernatant;
(3) make supernatant pass through to be filled with the chromatography post of resin extender, wash with water, to remove impurity, then with the alcohol-water solution eluting of higher concentration, collect eluent, concentrating under reduced pressure, dry, obtain Callicarpa plant extract.
7, the purposes according to technical scheme 6, wherein in step (1), extracting method is selected from homogenate extraction method, reflux extraction, ultrasonic extraction, microwave loss mechanisms and permeating extraction.
8, the purposes according to technical scheme 6 or 7, wherein in step (3), described resin extender is selected from macroporous adsorbent resin, polyamide and ion exchange resin.
9, the purposes according to any one of technical scheme 6-8, wherein in step (3), the alcohol-water solution of described higher concentration is the alcohol-water solution of 30 ~ 90 volume %.
10, the purposes according to any one of technical scheme 1-9, wherein said cosmetics are cream, frost, breast, liquid, powder or spray.
11, cosmetics, it contains the Callicarpa plant extract of 0.1 ~ 10.0%, preferably contain the Callicarpa plant extract of 0.5 ~ 5.0%, be more preferably the Callicarpa plant extract of 1.0 ~ 3.0%, the method preparation that described Callicarpa plant extract defines any one of technical scheme 6-9.
12, the cosmetics described in technical scheme 11 are cream, frost, breast, liquid, powder or spray.
Accompanying drawing explanation
Fig. 1 shows the removing situation of Folium Callicarpae Formosanae extract to hydroxyl radical free radical of variable concentrations, wherein: callicarpa cathayana Chang leaf extract, ◇: callicarpa pedunculata leaf extract, △: Callicarpa kwangtungensis Chun stem and leaf extract, and zero: Folium Callicarpae Macrophyllae stem extract ,+: vitamin C.
Fig. 2 shows the removing situation of Folium Callicarpae Formosanae extract to DPPH free radical of variable concentrations, wherein: callicarpa cathayana Chang leaf extract, ◇: callicarpa pedunculata leaf extract, △: Callicarpa kwangtungensis Chun stem and leaf extract, and zero: Folium Callicarpae Macrophyllae stem extract ,+: vitamin C.
Fig. 3 shows the free radical scavenging situation of Folium Callicarpae Formosanae extract to superoxide anion of variable concentrations, wherein: callicarpa cathayana Chang leaf extract, ◇: callicarpa pedunculata leaf extract, △: Callicarpa kwangtungensis Chun stem and leaf extract, and zero: Folium Callicarpae Macrophyllae stem extract ,+: vitamin C.
Fig. 4 shows the suppression situation of Folium Callicarpae Formosanae extract to tyrosinase activity of variable concentrations, wherein: callicarpa cathayana Chang leaf extract, ◇: callicarpa pedunculata leaf extract, △: Callicarpa kwangtungensis Chun stem and leaf extract, and zero: Folium Callicarpae Macrophyllae stem extract ,+: arbutin.
specific implementation method
The present inventor is surprised to find, Callicarpa plant extract has speckle dispelling, whitening, sun-proof, wrinkle removal or defying age purposes, utilizing Callicarpa plant to develop cosmetics, especially exploitation is used for speckle dispelling, whitening, sun-proof, wrinkle removal or antidotal cosmetics aspect and has broad prospects.
On the one hand, the invention provides Callicarpa plant extract and prepare the purposes in cosmetics.According to the present invention, Callicarpa plant extract is particularly useful for for the preparation of speckle dispelling, whitening, wrinkle removal, sun-proof or antidotal cosmetics.
According to the present invention, Callicarpa plant extract, by water extraction or alcohol extraction or water, alcohol mixed extraction method, is prepared by the stem of Verenaceae Callicarpa plant and/or leaf (being preferably dry stem and/or leaf).The limiting examples being applicable to Verenaceae Callicarpa plant of the present invention includes but not limited to sharp leaf Folium Callicarpae Formosanae (CallicarpaacutifoliaH.T.Chang), different leaf Folium Callicarpae Formosanae (Callicarpaanisophylla), wood Folium Callicarpae Formosanae (CallicarpaarboreaRoxb.Hort.Beng), Folium Callicarpae Formosanae (CallicarpabodinieriLevl.), Callicarpa brevipes (Benth.) Hance (Callicarpabrevipes (Benth.) Hance), Folium Callicarpae candicantis (Callicarpacandicans (Burm.f.) Hochr.), callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang), Jinyun Folium Callicarpae Formosanae (CallicarpachinyunensisP ' eietW.Z.Fang), hills Folium Callicarpae Formosanae (CallicarpacollinaDiels), multiple tooth Folium Callicarpae Formosanae (Callicarpadentosa (H.T.Chang) W.Z.Fang), Callicarpa dichotoma (Callicarpadichotoma (Lour) K.Koch), red body Folium Callicarpae Formosanae (CallicarpaerythrostictaMerr.etChun), callicarpa pedunculata (CallicarpaformosanaRolfe), Radix Callicarpae Giraldii (CallicarpagiraldiiHesseexRehd), Hubei Folium Callicarpae Formosanae (CallicarpagracilipesRehd), thick calyx Folium Callicarpae Formosanae (CallicarpahungtaiiP ' eietS.L.Chen), entire beautyberry herb (CallicarpaintegerrimaChamp), Japan Folium Callicarpae Formosanae (Callicarpajaponicathunb), callicarpa kochiana (CallicarpakochianaMakino), reddish tone Folium Callicarpae Formosanae (CallicarpakotoensisHayata), Callicarpa kwangtungensis Chun (CallicarpakwangtungensisChun), light leaf Folium Callicarpae Formosanae (CallicarpalingiiMerr), Callicarpa lobo-apiculata Metc. (CallicarpaloboapiculataMetc.), long luxuriant Folium Callicarpae Formosanae (CallicarpalongibracteataH.T.Chang), Folium Callicarpae Loureiri (CallicarpalongifoliaLamk.), long handle Folium Callicarpae Formosanae (CallicarpalongipesDunn), Folium Callicarpae Longissimae (Callicarpalongissima (Hemsl.) Merr.), yellow gland Folium Callicarpae Formosanae (CallicarpaluteopunctataH.T.Chang), Folium Callicarpae Macrophyllae (CallicarpamacrophyllaVahl), Callicarpa nudiflora (CallicarpanudifloraHook.), sieve floats Folium Callicarpae Formosanae (CallicarpaoliganthaMerr.), spend Folium Callicarpae Formosanae (CallicarpapaucifloraChunexH.T.Chang) less, glochild Folium Callicarpae Formosanae (CallicarpapeichienianaChenetS.L.Chen), rattan Folium Callicarpae Formosanae (CallicarpapeiiH.T.Chang), become mildewed Folium Callicarpae Formosanae (CallicarpapilosissimaMaxim.), Pingshan Folium Callicarpae Formosanae (CallicarpapingshanensisC.Y.WuexW.Z.Fang), white back of the body Folium Callicarpae Formosanae (CallicarpapoilaneiP.Dop), to sprout Folium Callicarpae Formosanae (CallicarpaproliferaC.Y.Wu), intend Folium Callicarpae Rubellae (CallicarpapseudorubellaH.T.Chang), the large Folium Callicarpae Formosanae of mountains in a range (CallicarparandaiensisHayata), dredge tooth Folium Callicarpae Formosanae (CallicarparemotiserrulataHayata), Folium Callicarpae Rubellae (CallicarparubellaLindl.), water JINHUA (CallicarpasalicifoliaP ' eietW.Z.Fang), upper lion Folium Callicarpae Formosanae (Callicarpasiong-saiensisMetc.), ancient cooking vessel lake Folium Callicarpae Formosanae (CallicarpatingwuensisH.T.Chang) and Yunnan Folium Callicarpae Formosanae (CallicarpayunnanensisW.Z.Fang).In a preferred embodiment, described Verenaceae Callicarpa plant is selected from callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang), callicarpa pedunculata (CallicarpaformosanaRolfe), Folium Callicarpae Macrophyllae (CallicarpamacrophyllaVahl) and Callicarpa kwangtungensis Chun (CallicarpakwangtungensisChun).
Particularly, the preparation method of Callicarpa plant extract, comprises the following steps:
(1) stem of Callicarpa plant and/or leaf (being preferably dry stem and/or leaf) are pulverized, with solvent extraction 1 ~ 3 time, described solvent is the mixture of water, ethanol or water and ethanol;
(2) each extracting solution is merged, the solvent described in concentrating under reduced pressure removing step (1); Add the water of 0.5 times ~ 2 times of volumes, hold over night, centrifugal or filtration obtains supernatant;
(3) make supernatant pass through to be filled with the chromatography post of resin extender, wash with water, to remove impurity, then with the alcohol-water solution eluting of higher concentration, collect eluent, concentrating under reduced pressure, dry, obtain Callicarpa plant extract.
In the above-mentioned methods, extracting method in step (1) is selected from homogenate extraction method, reflux extraction, ultrasonic extraction, microwave loss mechanisms and permeating extraction, wherein preferred homogenate extraction method, reflux extraction or permeating extraction, more preferably permeating extraction.
In the above-mentioned methods, the stem of the Callicarpa plant in step (1) and/or leaf, be preferably dry stem and/or leaf.Usually the stem of Callicarpa plant and/or leaf are ground into the coarse powder or most coarse powder that define in " Chinese Pharmacopoeia 2010 editions " note on the use.
In the above-mentioned methods, the mixture of the second alcohol and water in step (1) is preferably the ethanol water of 50 ~ 90 volume %, is more preferably the ethanol water of 70 ~ 90 volume %.
In the above-mentioned methods, the consumption of the solvent in step (1) is preferably 5 ~ 20 times amount of medical material (that is, 5 ~ 20ml solvent/g medical material), is more preferably 10 ~ 12 times amount (that is, 10 ~ 12ml flux/g medical material).
In the above-mentioned methods, in step (3), after concentrating under reduced pressure eluent, carry out following operation optional one or more time: using water dissolution concentrated solution, making it the chromatography post by being filled with resin extender, with solution washing, to remove impurity, then with the alcohol-water solution eluting of higher concentration, eluent is collected, concentrating under reduced pressure.
In the above-mentioned methods, the described resin extender in step (3) is selected from but is not limited to macroporous adsorbent resin, polyamide and ion exchange resin.In a kind of embodiment, described resin extender is preferably HPD100, HPD200, D101, AB-8, SP825, ADS-7 type macroporous adsorbent resin, is more preferably D101, AB-8 type macroporous adsorbent resin.
In one embodiment, in the above-mentioned methods, the aqueous solution of 2 ~ 8 times (6 times of preferred resin post bed volume) of resin column bed volume is used to wash in step (3).Resin column bed volume changes according to the amount of the pending supernatant of reality, and such as the ratio of resin column bed volume and pending supernatant volume can be about 1: 0.5 ~ 2.
In the above-mentioned methods, the alcohol-water solution of the higher concentration described in step (3) is the alcohol-water solution of 30 ~ 90 volume %, be preferably the alcohol-water solution of 30 ~ 80 volume %, be more preferably the alcohol-water solution of 30 ~ 70 volume %, be more preferably the alcohol-water solution of 30 ~ 50 volume %.Its consumption is 2 ~ 5 times of resin column bed volume, is preferably 3 ~ 4 times of resin column bed volume.Resin column bed volume changes according to the amount of the pending supernatant of reality, and such as the ratio of resin column bed volume and pending supernatant volume can be about 1: 0.5 ~ 2.In a kind of embodiment, described alcohol is preferably ethanol.
By adjuvant additive combination acceptable on Callicarpa plant extract of the present invention and cosmetics, thus can make for speckle dispelling, whitening, wrinkle removal, sun-proof or anti-ageing aging cosmetics.As required, described cosmetics can be made any form that cosmetics allow, such as but be not restricted to cream, frost, breast, liquid, powder or spray.According to the present invention, described cosmetics contain 0.1 ~ 10.0% Callicarpa plant extract, preferably containing 0.5 ~ 5.0% Callicarpa plant extract, more preferably containing 1.0 ~ 3.0% Callicarpa plant extracts.
Be applicable to acceptable auxiliary additive on the cosmetics in cosmetics of the present invention and include but not limited to binding agent, lubricant, disintegrating agent, correctives, antioxidant, emulsifying agent, thickening agent, antiseptic etc.
Above-mentioned binding agent includes but not limited to hydroxypropyl cellulose, corn starch, pregelatinized Starch, modified corn starch, polyvinylpyrrolidone, hydroxypropyl emthylcellulose, lactose, arabic gum, ethyl cellulose, cellulose acetate etc.
Above-mentioned lubricant includes but not limited to magnesium stearate, zinc stearate, calcium stearate, Talcum, stearic acid, silica sol, Palmic acid etc.
Above-mentioned disintegrating agent includes but not limited to cross-linking sodium carboxymethyl cellulose, crospolyvinylpyrrolidone, starch, potato starch, pregelatinized Starch, corn starch, primojel, microcrystalline Cellulose, hydroxypropyl cellulose etc.
Above-mentioned correctives includes but not limited to fruit essence, plant essence etc.
Above-mentioned antioxidant includes but not limited to anti-butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), propyl gallate (PG), ascorbic acid, alpha-tocopherol etc.
Mentioned emulsifier includes but not limited to arabic gum, sodium alkyl benzene sulfonate, sodium stearoyl lactate etc.
Above-mentioned thickening agent includes but not limited to methylcellulose, carboxymethyl cellulose, hydroxypropyl cellulose, agar, sodium alginate, gelatin etc.
Foregoing preservatives includes but not limited to potassium sorbate, sodium benzoate, parabens etc.
Beneficial effect
1, simple according to the extraction process of Callicarpa plant extract of the present invention, and the raw material Callicarpa plant origin used is extensive, use with a long history, economic and practical, safety is high;
2, according to Callicarpa plant extract of the present invention can effectively scavenging free radicals, effectively restraint of tyrosinase active, effectively reduce ultra-violet absorption and effectively to anti aging effect.
Embodiment
Be illustrated the present invention by the following examples, following examples limit the invention never in any form.
In following examples, callicarpa cathayana Chang and the Flos Carthami place of production are Hubei, and the place of production of Callicarpa kwangtungensis Chun and Folium Callicarpae Macrophyllae is Guangdong, and the dried leaves of each medical material and stem are crushed to most coarse powder (its definition is see Chinese Pharmacopoeia 2010 editions second notes on the use).Extracting flash extracter used is JHBE-50 type, purchased from Henan Jinnai Technology Development Co., Ltd..D101, HPD100, AS-7 macroporous adsorbent resin is all purchased from Cangzhou, Hebei Bao En Chemical Co., Ltd..Polyamide (80 ~ 120 order), purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
Except as otherwise noted, the alcoholic solution in following examples refers to ethanol water, and with volume percentage.
Except as otherwise noted, in following examples, term " concentrated solution volume is suitable with medical material amount " refers to that the amount of the amount (in ml) of concentrated liquid and original medical material is (in g) equal; Resin column bed volume be the 2-0.5 of pending supernatant volume doubly.
In following examples, centrifugal condition is 5000rpm, about 10 minutes.
Embodiment 1
The dried leaves of callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang) is crushed to most coarse powder, with the flow velocity seepage pressure effects 10h of 90% ethanol by every gram of callicarpa cathayana Chang dried leaves coarse powder 1mL/h.Collect percolate, concentrating under reduced pressure percolate, to remove ethanol, concentrated solution volume is suitable with medical material amount.Double the water of volume, hold over night, centrifugally obtains supernatant.Make supernatant by D101 macroporous adsorptive resins, with the water washing impurity of 6 times of resin column bed volume amounts, discard water lotion, then carry out eluting with 40% ethanol of 3 times of resin column bed volume amounts, collect eluent.Concentrating under reduced pressure eluent, to remove ethanol.With water, concentrated solution is diluted to initial supernatant liquid to amass, then by polyamide chromatography post, with the water washing of 2 times of resin column bed volume amounts, discard water lotion, then use 40% ethanol elution of 3 times of resin column bed volume amounts, collect eluent, by eluent concentrating under reduced pressure, drying, obtains callicarpa cathayana Chang leaf extract, is sepia uniform powder.
Embodiment 2
The dry stem of callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang) and leaf are crushed to most coarse powder, add 12 times amount (namely, the dry stem of 12ml/g callicarpa cathayana Chang and leaf powder) 80% ethanol, homogenate extraction 3min, extract 2 times, merge extractive liquid, concentrating under reduced pressure is to remove ethanol, and concentrated solution volume is suitable with medical material amount.Double the water of volume, hold over night, centrifugally obtains supernatant.Make supernatant by D101 macroporous adsorptive resins, with the water washing of 6 times of resin column bed volume amounts, discard water lotion, carry out eluting with 30% ethanol of 3 times of resin column bed volume amounts, collect eluent.By eluent concentrating under reduced pressure, removing ethanol.With water, concentrated solution is diluted to initial supernatant liquid to amass, then by polyamide chromatography post, with the water washing of 2 times of resin column bed volume amounts, discard water lotion, then use 30% ethanol elution of 3 times of resin column bed volume amounts, collect eluent, by eluent concentrating under reduced pressure, drying, obtains callicarpa cathayana Chang stem and leaf extract, is sepia uniform powder.
Embodiment 3
The dried leaves of callicarpa pedunculata (CallicarpaformosanaRolfe) is crushed to most coarse powder, add 70% ethanol of 12 times amount (that is, 12ml/g callicarpa pedunculata dried leaves powder), homogenate extraction 3min, extraction time is 2 times.Merge extracted twice thing, concentrating under reduced pressure extracting solution, to remove ethanol, concentrated solution volume is suitable with medical material amount.Double the water of volume, hold over night, centrifugally obtains supernatant.Make supernatant by D101 macroporous adsorptive resins, with the water washing of 6 times of resin column bed volume amounts, discard water lotion, carry out eluting with 30% ethanol of 4 times of resin column bed volume amounts, collect eluent.By eluent concentrating under reduced pressure, dry, obtaining callicarpa pedunculata leaf extract, is sepia uniform powder.
Embodiment 4
The dry stem of callicarpa pedunculata (CallicarpaformosanaRolfe) and leaf are crushed to most coarse powder, add 12 times amount (namely, the dry stem of 12ml/g callicarpa pedunculata and leaf powder) 70% ethanol, backflow (being heated to boiling under normal pressure) decocts 1h, and decocting number of times is 2 times.Merge twice and decoct extracting solution, concentrating under reduced pressure extracting solution, to remove ethanol, concentrated solution volume is suitable with medical material amount.Double the water of volume, hold over night, centrifugally obtains supernatant.Make supernatant by HPD100 macroporous adsorptive resins, with the water washing of 6 times of resin column bed volume amounts, discard water lotion, with 40% ethanol elution of 3 times of resin column bed volume amounts, collect eluent.Concentrating under reduced pressure eluent, to remove ethanol.With water, concentrated solution is diluted to initial supernatant liquid to amass, then by ADS-7 resin column, with the water washing of 3 times of resin column bed volume amounts, discards water lotion, then carry out eluting with 50% ethanol of 3 times of resin column bed volume amounts, collect eluent.By eluent concentrating under reduced pressure, dry, obtaining callicarpa pedunculata stem and leaf extract, is sepia uniform powder.
Embodiment 5
The dry stem of Callicarpa kwangtungensis Chun (CallicarpakwangtungensisChun) and leaf are crushed to most coarse powder, with the flow velocity seepage pressure effects 10h of 90% ethanol by the dry stem of every gram of Callicarpa kwangtungensis Chun and leaf powder 1mL/h.Collect percolate, concentrating under reduced pressure percolate, to remove ethanol, concentrated solution volume is suitable with medical material amount.Double the water of volume, hold over night, centrifugally obtains supernatant.Make supernatant by D101 macroporous adsorptive resins, with the water washing impurity of 6 times of resin column bed volume amounts, discard water lotion, then carry out eluting with 70% ethanol of 3 times of resin column bed volume amounts, collect eluent.By eluent concentrating under reduced pressure, dry, obtaining Callicarpa kwangtungensis Chun stem and leaf extract, is sepia uniform powder.
Embodiment 6
The dry stem of Folium Callicarpae Macrophyllae (CallicarpamacrophyllaVahl.) is crushed to most coarse powder, add 10 times amount (namely, the dry stem powder of 10ml/g Folium Callicarpae Macrophyllae) 90% ethanol, backflow (being heated to boiling under normal pressure) decocts 1h, and decocting number of times is 2 times.Merge twice and decoct extracting solution, concentrating under reduced pressure extracting solution, to remove ethanol, concentrated solution volume is suitable with medical material amount.Double the water of volume, hold over night, centrifugally obtains supernatant.Make supernatant by D101 macroporous adsorptive resins, with the water washing of 3 times of resin column bed volume amounts, discard water lotion, then with 80% ethanol elution of 3 times of resin column bed volume amounts, collect eluent.By eluent concentrating under reduced pressure, dry, obtaining Folium Callicarpae Macrophyllae stem extract, is sepia uniform powder.
Embodiment 7
Callicarpa plant extract of the present invention is studied the Scavenging activity of free radical (hydroxyl radical free radical, DPPH free radical and superoxide anion).
1 instrument and reagent
1.1 instrument
Thermostat water bath, model HH-S11-2, purchased from Chang'an, Beijing scientific instrument factory; Ultraviolet-uisible spectrophotometer, model TU-1800PC/TU-1800SPC is purchased from Beijing Puxi General Instrument Co., Ltd;
1.2 reagent
1,1 diphenyl-2-trinitrophenyl-hydrazine (DPPH), purchased from sigma company; Salicylic acid, purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Pyrogallol, purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Hydrogen peroxide, purchased from Chemical Reagent Co., Ltd., Sinopharm Group; FeSO
4, purchased from Chemical Reagent Co., Ltd., Sinopharm Group; The Tris-HCl buffer of 0.05mol/LpH8.2, purchased from grinding territory (Shanghai) chemical reagent company limited; All the other reagent are domestic chemically pure reagent.
1.3 sample
Callicarpa cathayana Chang leaf extract, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract are prepared according to embodiment 1,3,5,6 respectively; Vitamin C, purchased from lark prestige Science and Technology Ltd..
2 experimental techniques
2.1 Hydroxyl radical-scavenging tests
Prepare the FeSO of 9mmol/L successively
4, 8.8mmol/LH
2o
2and 9mmol/L salicylic acid.
Test sample solution preparation: compound concentration is the callicarpa cathayana Chang leaf extract of 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.8mg/mL and 1.0mg/mL, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract, Folium Callicarpae Macrophyllae stem extract and ascorbic aqueous solution successively.
The FeSO of 2mL is added successively in color comparison tube
4, 2mL salicylic acid, 2mL aqueous solution and 2mLH
2o
2, shake up; Take out after 37 DEG C of heating in water bath 30min, survey its absorbance A at 510nm place
0; The FeSO of 2mL is added successively in color comparison tube
4, 2mL salicylic acid, the test sample of 2mL variable concentrations and 2mLH
2o
2, shake up; Take out after 37 DEG C of heating in water bath 30min, survey its absorbance A at 510nm place
1; The FeSO of 2mL is added successively in color comparison tube
4, 2mL salicylic acid, the test sample of 2mL variable concentrations and 2mL aqueous solution, shake up, take out after 37 DEG C of heating in water bath 30min, survey its absorbance A at 510nm place
2; According to following formulae discovery test sample to the clearance rate of OH:
OH clearance rate (%)=100 × (A
0-(A
1-A
2))/A
0
Hydroxyl radical-scavenging result of the test is see accompanying drawing 1.More high anti-oxidation ability is stronger for clearance rate.
2.2DPPH free radical scavenging is tested
Accurately take 7.88mgDPPH, with anhydrous alcohol solution and standardize solution in 100mL volumetric flask, DPPH concentration is 2 × 10
-4mo1/L, keep in Dark Place (0 ~ 4 DEG C).
Test sample solution preparation: compound concentration is the callicarpa cathayana Chang leaf extract of 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.8mg/mL and 1.0mg/mL, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract, Folium Callicarpae Macrophyllae stem extract and ascorbic aqueous solution successively.
Respectively by 2mLDPPH alcoholic solution and 2mL aqueous solution, the test sample aqueous solution of 2mL variable concentrations and the test sample aqueous solution of the DPPH alcoholic solution of 2mL and 2mL variable concentrations and the aqueous solution Homogeneous phase mixing of 2mL, place 30min in the dark, with 50% ethanol for blank measures its absorbance A i, Aj and Ac at 525nm place, and according to following formulae discovery test sample to the clearance rate of DPPH free radical:
Clearance rate (%)=[1-(Ai-Aj)/Ac] × 100%
In formula: the absorbance of Ac:2mLDPPH alcoholic solution+2mL aqueous solution; Ai:2mL tests the absorbance of sample aqueous solution+2mLDPPH alcoholic solution; Aj:2mL tests the absorbance of sample aqueous solution+2mL aqueous solution.
DPPH free radical scavenging result of the test is see accompanying drawing 2, and more high anti-oxidation ability is stronger for clearance rate.
2.3 superoxide anion clearance tests
Preparation of reagents: the Tris-HCL buffer of 0.05mol/L, pH8.2; The HCL solution of 10nmol/L; The HCL solution of 8mol/L; Pyrogallol-10mmol/LHCL the solution (the 3mmol/L pyrogallol solution prepared with the HCL of 10mmol/L) of 3mmol/L
Test sample solution preparation: compound concentration is the callicarpa cathayana Chang leaf extract of 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.8mg/mL and 1.0mg/mL, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract, Folium Callicarpae Macrophyllae stem extract and ascorbic aqueous solution successively.
The Tris-HCl buffer getting 4.5mL, in test tube, is placed in 25 DEG C of water-bath preheatings; Add 4.2mL aqueous solution, be placed in 25 DEG C of water-baths and be incubated 20min, adding 0.3mL concentration after taking-up is immediately 3mmol/L pyrogallol solution (preheating in 25 DEG C of water-baths), shake up, add rapidly in color comparison tube, add the HCL solution stopped reaction that 1.0mL concentration is 8mol/L after reaction 5min, measure absorbance A at 325nm place
0.
The Tris-HCl buffer getting 4.5mL, in test tube, is placed in 25 DEG C of water-bath preheatings; Add the test sample aqueous solution of 4.2mL variable concentrations, be placed in 25 DEG C of water-baths and be incubated 20min, adding 0.3mL concentration after taking-up is immediately 3mmol/L pyrogallol solution (preheating in 25 DEG C of water-baths), shake up, add rapidly in color comparison tube, add the HCL solution stopped reaction that 1.0mL concentration is 8mol/L after reaction 5min, measure absorbance A at 325nm place
1.
The Tris-HCl buffer getting 4.5mL, in test tube, is placed in 25 DEG C of water-bath preheatings; Add the test sample aqueous solution of 4.2mL variable concentrations, be placed in 25 DEG C of water-baths and be incubated 20min, to add 0.3mL concentration after taking-up be immediately 3mmol/L concentration is the HCL solution (preheating in 25 DEG C of water-baths) of 10mmol/L, shake up, add rapidly in color comparison tube, add the HCL solution stopped reaction that 1.0mL concentration is 8mol/L after reaction 5min, measure absorbance A at 325nm place
2.
Clearance rate (%)=100 × (A
0-(A
1-A
2))/A
0
In formula: A
0for the absorbance of aqueous solution+pyrogallol, A
1for testing the absorbance of sample aqueous solution+pyrogallol solution; A
2for the absorbance of test sample aqueous solution+10mmol/LHCL solution.
Superoxide anion clearance test result is see accompanying drawing 3.More high anti-oxidation ability is stronger for clearance rate.
3 result of the tests
Conventional oxidation resistance evaluation methodology to the Scavenging activity of hydroxyl radical free radical, DPPH free radical, ultra-oxygen anion free radical.1 ~ 3 is the results are shown in Figure according to the removing to hydroxyl radical free radical, DPPH free radical, ultra-oxygen anion free radical of callicarpa cathayana Chang leaf extract of the present invention, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract.As Figure 1-3, along with the increase of concentration, each Folium Callicarpae Formosanae extract and positive control vitamin C increase free radical scavenging activity, callicarpa cathayana Chang leaf extract and the Scavenging activity of callicarpa pedunculata leaf extract to three kinds of free radicals are better than positive control vitamin C, and the ability of Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract scavenging free radicals is suitable with positive control vitamin C.Conclusion: callicarpa cathayana Chang leaf extract, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract all have stronger oxidation resistance, and wherein the oxidation resistance of callicarpa cathayana Chang leaf extract is the strongest.
Embodiment 8
Callicarpa plant extract of the present invention is studied the rejection ability of tyrosinase activity.
1 instrument and reagent
1.1 instrument
Ultraviolet-uisible spectrophotometer, model TU-1800PC/TU-1800SPC, purchased from Beijing Puxi General Instrument Co., Ltd; Electronic analytical balance, BT25S, purchased from Sai Duolisi scientific instrument (Beijing) company limited; DZF-6050 vacuum drying oven (the upper grand testing equipment company limited of Nereid).
1.2 reagent
PBS buffer: the buffer being mixed with pH=6.85 by pharmacopeia; TYR, purchased from Chemical Reagent Co., Ltd., Sinopharm Group, is mixed with the aqueous solution that concentration is 0.1%; Mushroom Tyrosinase, purchased from American sigma company, is mixed with the aqueous solution of 0.05mg/mL; Water is deionized water; All the other reagent are domestic analytical pure.
1.3 sample
Callicarpa cathayana Chang leaf extract, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract are prepared according to embodiment 1,3,5,6 respectively; Arbutin, purchased from Aladdin reagent (Shanghai) Co., Ltd..
2 experimental techniques
Draw 0.5mLL-tryrosinase aqueous solution, 2.0mLPBS buffer, mixing, is placed in 37 DEG C of water-bath constant temperature 30min, then adds 0.5mL Mushroom Tyrosinase solution, mixing, after reaction 10min, determines absorbance A in 475nm place
1.
Draw 2.5mLPBS buffer, be placed in 37 DEG C of water-bath constant temperature 30min, then add 0.5mL Mushroom Tyrosinase solution, mixing, after reaction 10min, determine absorbance A in 475nm place
2.
Draw 0.5mLL-tryrosinase aqueous solution, the test sample aqueous solution of 0.5mL variable concentrations, 1.5mLPBS buffer, mixing, is placed in 37 DEG C of water-bath constant temperature 30min, add 0.5mL Mushroom Tyrosinase solution again, mixing, after reaction 10min, determines absorbance A in 475nm place
3.
Draw the test of 0.5mL variable concentrations sample aqueous solution, 2.0mLPBS buffer, mixing, is placed in 37 DEG C of water-bath constant temperature 30min, then adds 0.5mL Mushroom Tyrosinase solution, mixing, after reaction 10min, determines absorbance A in 475nm place
4.
According to following formulae discovery Folium Callicarpae Formosanae extract of the present invention to the suppression ratio of tryrosinase:
Suppression ratio (%)=[1-(A
3-A
4)/(A
1-A
2)] × 100%
In formula: A
1: the absorbance of contrast solution (TYR aqueous solution+Mushroom Tyrosinase aqueous solution+PBS buffer)
A
2: the absorbance of contrast blank solution (Mushroom Tyrosinase aqueous solution+PBS buffer)
A
3: the absorbance of test sample solution (TYR aqueous solution+Mushroom Tyrosinase aqueous solution+test sample aqueous solution+PBS buffer)
A
4: the absorbance of test sample blank solution (Mushroom Tyrosinase aqueous solution+test sample aqueous solution+PBS buffer)
In this test the sample of test be prepare according to embodiment 1,3,5,6 callicarpa cathayana Chang leaf extract, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract and arbutin aqueous solution, test concentrations is respectively 0.2mg/mL, 0.4mg/mL, 0.8mg/mL, 1.2mg/mL, 1.6mg/mL, 2.0mg/mL, 2.5mg/mL, 5.0mg/mL, 10.0mg/mL.
3 result of the tests
Restraint of tyrosinase activity experiment is conventional whitening, speckle dispelling merit rating method.Callicarpa cathayana Chang leaf extract, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract and the suppression situation of positive control arbutin to tyrosinase activity are shown in Fig. 4.As shown in Figure 4, along with the increase of concentration, each Folium Callicarpae Formosanae extract and positive control arbutin increase the suppression ratio of tyrosinase activity, wherein the ability of callicarpa cathayana Chang leaf extract and callicarpa pedunculata leaf extract restraint of tyrosinase activity is better than positive control arbutin, and Callicarpa kwangtungensis Chun stem and leaf extract is suitable with positive control arbutin with Folium Callicarpae Macrophyllae stem extract.Conclusion: it is active that Folium Callicarpae Formosanae extract all has stronger restraint of tyrosinase, can reach the effect of speckle dispelling, whitening by restraint of tyrosinase activity.
Embodiment 9
Callicarpa plant extract ultraviolet absorption ability research of the present invention.
1 instrument and reagent
1.1 instrument
Ultraviolet-uisible spectrophotometer, model TU-1800PC/TU-1800SPC, purchased from Beijing Puxi General Instrument Co., Ltd; Electronic analytical balance, BT25S, purchased from Sai Duolisi scientific instrument (Beijing) company limited.
1.2 reagent
Ethanol, purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
2 experimental techniques
2.1 detection method
Sample (callicarpa cathayana Chang leaf extract, callicarpa pedunculata leaf extract, Callicarpa kwangtungensis Chun stem and leaf extract and Folium Callicarpae Macrophyllae stem extract respectively according to embodiment 1,3,5,6 prepare) will be tested with 50% ethanol water to be diluted to every milliliter and to be equivalent to crude drug 0.5mg, with 50% ethanol water for blank, scan in 200-400nm wave-length coverage, measure the light transmittance under each wavelength, measure wavelength by following subregion:
UV-C district (short wave ultraviolet district, 200-280nm) 200,210,220,230,240,250,260,270,280nm;
UV-B district (ultraviolet B radiation district, 280-320nm) 280,290,300,310,320nm;
UV-A district (long wave ultraviolet district, 320-400nm) 320,330,340,350,360,370,380,390,400nm.
2.2 evaluation methodology
Absorption of UV=100%-light transmittance.
Absorption of UV is person more than 80%, can think to have anti-sunlight function; Absorption of UV is person more than 90%, can think that anti-sunlight function is stronger.
3 result of the tests
Test sample the results are shown in following table 1 to different wave length absorption of UV:
UV-C, UV-B, UV-A absorption of UV of table 1 Callicarpa plant extract matter sample
Ultraviolet absorption ability is conventional sun-proof merit rating method.Result show, callicarpa cathayana Chang extract, callicarpa pedunculata extract to the ultraviolet absorption ability of different wave length all more than 90%, Callicarpa kwangtungensis Chun extract and Folium Callicarpae Macrophyllae extract to the ultraviolet absorption ability of different wave length also all more than 80%.Conclusion: Callicarpa plant extract effectively can reduce ultra-violet absorption is desirable broad spectrum sunscreen.
Embodiment 10
Callicarpa plant extract of the present invention is to anti aging effect Effect study.
1 instrument and reagent
1.1 instrument
Homogenizer, JYT-10 type, purchased from Shanghai FLUKO company.
1.2 reagent
D-galactose, purchased from actual two factories in Shanghai; Sodium sulfide barbiturates, available from Sigma; Ethanol, glycerol, purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Polyoxyethylene (2) stearic alcohol ether, polyoxyethylene (21) stearic alcohol ether, chemical grade, purchased from He great Chemical Company; Iso-octyl palmitate, dimethicone, Jojoba oil, cetearyl alcohol, glyceryl monostearate, methyl hydroxybenzoate, chemical grade, purchased from Shanghai Lisheng Co., Ltd.; SOD test kit, HYP test kit and MDA kit reagent box build up bio-engineering corporation purchased from Nanjing.
1.3 sample
According to callicarpa cathayana Chang leaf extract prepared by embodiment 1.
1.4 animal
3 monthly age cleaning grade Kunming Female nude mice (University Of Suzhou's medical college Experimental Animal Center), average weight 30 ± 2g, standard feed is raised.
2 experimental techniques
The preparation of 2.1 test cosmetics
The formula of test cosmetics sees the following form 2.
Table 2 callicarpa cathayana Chang leaf extract cosmetic formulations
| Raw material | Composition (quality %) |
| Callicarpa cathayana Chang leaf extract | 2.0 |
| Polyoxyethylene (2) stearic alcohol ether | 2.5 |
| Polyoxyethylene (21) stearic alcohol ether | 1.5 |
| Jojoba oil | 4.0 |
| Cetearyl alcohol | 3.0 |
| Glyceryl monostearate | 2.5 |
| Stearic acid | 0.2 |
| Iso-octyl palmitate | 0.2 |
| Ethanol | 0.5 |
| Methyl hydroxybenzoate | 0.5 |
| Water | Surplus |
By polyoxyethylene (2) stearic alcohol ether, polyoxyethylene (21) stearic alcohol ether, Jojoba oil, cetearyl alcohol, glyceryl monostearate, stearic acid mixing post-heating to 90 DEG C stirring, be incubated for subsequent use as A phase; Iso-octyl palmitate is dissolved in deionized water, is heated to 90 DEG C and is incubated for subsequent use as B phase; Callicarpa cathayana Chang leaf extract is added water and ethanol in proper amount dissolving, as C phase; When biphase temperature is roughly the same, under homogenizer state, B phase is slowly added A phase, continue homogenizing about 5min with homogenizer simultaneously; Then control temperature is at about 75 DEG C insulated and stirred froth breakings, when system temperature is down to 35 DEG C, adds C phase, adds methyl hydroxybenzoate simultaneously, continues slowly to stir, and discharging during room temperature loads in the bottle of having sterilized, to obtain final product.
2.2 animal groupings, administration and modeling
30 nude mices are divided into 3 groups at random, often organize 10.Blank group normal condition is raised, and does not inject and photo-irradiation treatment; Model group neck every day dorsal sc injection (sc) D-galactose 1000mg/kgd, stick with paste with 15% sodium sulfide simultaneously and slough back by hair and part horny layer, expose the skin of about 3cm × 5cm, with long wavelength (365nm) and short wavelength (254nm) ultraviolet radiation skin of back, UVA cumulative exposure intensity is 259.5J/cm
2, short wavelength's cumulative exposure intensity is 6.482J/cm
2.Experimental group injection and illumination basis on smear test cosmetics to its back again, every day 2 times, 0.2g/ time.
Continuous injection of d-galactose and illumination 6 weeks, treat that model group is slow in action, back wrinkle is obvious, present obvious old and feeble sign, model group and experimental group all stop injection of d-galactose and illumination, and experimental group stops smearing cosmetics simultaneously, puts to death all animals after 2 days.
The preparation of 2.3 skin histology homogenate (10%)
Get nude mice back skin tissues block about 1g, through pre-cold saline rinsing, removing subcutaneous fat and other connective tissues, filter paper is wiped dry, weigh, graduated cylinder measures the normal saline of this tissue 9 times of weight, get 2/3 to pour into and be equipped with in the burning mortar of piece of tissue, ophthalmology is little shred after, after grinding 15min, thick homogenate is poured in small beaker, with the normal saline flushing mortar of residue 1/3, 3min is pulverized continuously with in Ultrasonic Pulverization instrument (intensity 25%) ice bath, then multigelation 3 times, cellular content is free in liquid phase completely, by tissue homogenate at 3500r/min centrifugal 15 minutes, get supernatant.
The mensuration of SOD vigor, HYP content and MDA content in 2.4 skin histology homogenate
SOD vigor, HYP content and MDA content in bio-engineering corporation SOD (superoxide dismutase), HYP (hydroxyproline) and the homogenate of MDA (malonaldehyde) test kit description method mensuration skin histology is built up with reference to Nanjing.
3 experimental results
Nude mice skin organizes the measurement result of Biochemical Indexes to see the following form 3:
Table 3 nude mice skin organizes the measurement result of Biochemical Indexes
n=10)
| Group | SOD(U/mL) | HYP(μg/mL) | MDA(nmol/mL) |
| Blank group | 120.59±6.20＊＊ | 1.49±0.18＊＊ | 15.42±4.96＊＊ |
| Model group | 81.23±4.15 | 0.88±0.18 | 55.48±6.89 |
| Experimental group | 118.13±5.78＊＊ | 1.21±0.29＊ & | 12.42±3.41＊＊ & |
Note: compare with model group, * p < 0.05, * * p < 0.01; Compare with blank group,
aMP.AMp.Ampp < 0.05.
HYP content, SOD activity and MDA (malonaldehyde) content are conventional defying age indexes of capability evaluation.Result shows, and Folium Callicarpae Formosanae extract can improve HYP content and SOD activity in subacute aging and photoaging model nude mice skin tissue, and can reduce MDA content.Conclusion: Folium Callicarpae Formosanae extract has the function of anti aging effect.
The description of the above-described embodiment and examples of the present invention, only for the object explained and illustrate, not limits the present invention by any way.Clearly, those skilled in the art can carry out multiple change and change according to the instruction of the context of the invention.These are changed and change all drops in the spirit and scope of the invention that claim limits.
Claims (11)
1. Callicarpa plant extract is for the preparation of the purposes in speckle dispelling, whitening, wrinkle removal, sun-proof or anti-aging cosmetics.
2. purposes according to claim 1, wherein by weight, described cosmetics contain 0.1-10.0% Callicarpa plant extract.
3. purposes according to claim 1 and 2, wherein said Callicarpa plant extract is prepared by the stem of Verenaceae Callicarpa plant and/or leaf.
4. purposes according to claim 3, wherein said Verenaceae Callicarpa plant is selected from sharp leaf Folium Callicarpae Formosanae (CallicarpaacutifoliaH.T.Chang), different leaf Folium Callicarpae Formosanae (Callicarpaanisophylla), wood Folium Callicarpae Formosanae (CallicarpaarboreaRoxb.Hort.Beng), Folium Callicarpae Formosanae (CallicarpabodinieriLevl.), Callicarpa brevipes (Benth.) Hance (Callicarpabrevipes (Benth.) Hance), Folium Callicarpae candicantis (Callicarpacandicans (Burm.f.) Hochr.), callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang), Jinyun Folium Callicarpae Formosanae (CailicarpachinyunensisP ' eietW.Z.Fang), hills Folium Callicarpae Formosanae (CallicarpacollinaDiels), multiple tooth Folium Callicarpae Formosanae (Callicarpadentosa (H.T.Chang) W.Z.Fang), Callicarpa dichotoma (Callicarpadichotoma (Lour) K.Koch), red body Folium Callicarpae Formosanae (CallicarpaerythrostictaMerr.etChun), callicarpa pedunculata (CallicarpaformosanaRolfe), Radix Callicarpae Giraldii (CallicarpagiraldiiHesseexRehd), Hubei Folium Callicarpae Formosanae (CallicarpagracilipesRehd), thick calyx Folium Callicarpae Formosanae (CallicarpahungtaiiP ' eietS.L.Chen), entire beautyberry herb (CallicarpaintegerrimaChamp), Japan Folium Callicarpae Formosanae (CallicarpajaponicaThunb), callicarpa kochiana (CallicarpakochianaMakino), reddish tone Folium Callicarpae Formosanae (CallicarpakotoensisHayata), Callicarpa kwangtungensis Chun (CallicarpakwangtungensisChun), light leaf Folium Callicarpae Formosanae (CallicarpalingiiMerr), Callicarpa lobo-apiculata Metc. (CallicarpaloboapiculataMetc.), long luxuriant Folium Callicarpae Formosanae (CallicarpalongibracteataH.T.Chang), Folium Callicarpae Loureiri (CallicarpalongifoliaLamk.), long handle Folium Callicarpae Formosanae (CallicarpalongipesDunn), Folium Callicarpae Longissimae (Callicarpalongissima (Hemsl.) Merr.), yellow gland Folium Callicarpae Formosanae (CallicarpaluteopunctataH.T.Chang), Folium Callicarpae Macrophyllae (CallicarpamacrophyllaVahl), Callicarpa nudiflora (CallicarpanudifloraHook.), sieve floats Folium Callicarpae Formosanae (CallicarpaoliganthaMerr.), spend Folium Callicarpae Formosanae (CallicarpapaucifloraChunesH.T.Chang) less, glochild Folium Callicarpae Formosanae (CallicarpapeichienianaChunetS.L.Chen), rattan Folium Callicarpae Formosanae (CallicarpapeiiH.T.Chang), become mildewed Folium Callicarpae Formosanae (CallicarpapilosissimaMaxim.), Pingshan Folium Callicarpae Formosanae (CallicarpapingshanensisC.Y.WuexW.Z.Fang), white back of the body Folium Callicarpae Formosanae (CallicarpapoilaneiP.Dop), to sprout Folium Callicarpae Formosanae (CallicarpaproliferaC.Y.Wu), intend Folium Callicarpae Rubellae (CallicarpapseudorubellaH.T.Chang), the large Folium Callicarpae Formosanae of mountains in a range (CallicarparandaiensisHayata), dredge tooth Folium Callicarpae Formosanae (CallicarparemotiserrulataHayata), Folium Callicarpae Rubellae (CallicarparubellaLindl.), water JINHUA (CallicarpasalicifoliaP ' eietW.Z.Fang), upper lion Folium Callicarpae Formosanae (Callicarpasiong-saiensisMetc.), ancient cooking vessel lake Folium Callicarpae Formosanae (CallicarpatingwuensisH.T.Chang) and Yunnan Folium Callicarpae Formosanae (CallicarpayunnanensisW.Z.Fang).
5. purposes according to claim 3, wherein said Verenaceae Callicarpa plant is selected from callicarpa cathayana Chang (CallicarpacathayanaH.T.Chang), callicarpa pedunculata (CallicarpaformosanaRolfe), Folium Callicarpae Macrophyllae (CallicarpamacrophyllaVahl) and Callicarpa kwangtungensis Chun (CallicarpakwangtungensisChun).
6. the purposes according to any one of claim 1-3, wherein said Callicarpa plant extract is prepared by the method comprised the following steps:
(1) stem of Callicarpa plant and/or leaf are pulverized, with solvent extraction 1 ~ 3 time, described solvent is the mixture of water, ethanol or water and ethanol;
(2) each extracting solution is merged, the solvent described in concentrating under reduced pressure removing step (1); Add the water of 0.5 times ~ 2 times of volumes, hold over night, centrifugal or filtration obtains supernatant;
(3) make supernatant pass through to be filled with the chromatography post of resin extender, wash with water, to remove impurity, then with the alcohol-water solution eluting of higher concentration, collect eluent, concentrating under reduced pressure, dry, obtain Callicarpa plant extract.
7. purposes according to claim 6, wherein in step (1), extracting method is selected from homogenate extraction method, reflux extraction, microwave loss mechanisms, ultrasonic extraction and permeating extraction.
8. purposes according to claim 6, wherein in step (3), described resin extender is selected from macroporous adsorbent resin, polyamide and ion exchange resin.
9. purposes according to claim 6, wherein in step (3), the alcohol-water solution of described higher concentration is the alcohol-water solution of 30% ~ 90 volume %.
10. the purposes according to any one of claim 1-9, wherein said cosmetics are cream, frost, breast, liquid, powder or spray.
11. cosmetics, it contains the Callicarpa plant extract of 0.1-10.0%, the method preparation that described Callicarpa plant extract defines any one of claim 6-9.
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| CN105943436A (en) * | 2016-05-29 | 2016-09-21 | 徐国财 | Anti-ultraviolet and anti-aging skin care product and preparation method thereof |
| CN107669531A (en) * | 2016-12-12 | 2018-02-09 | 青岛大学 | A kind of pale spot skin cosmetics |
| CN109007439A (en) * | 2018-07-25 | 2018-12-18 | 广州格雷特生物科技有限公司 | Containing callicarpa nudiflora prawn feed additive and its preparation method and application |
| CN110314114A (en) * | 2018-03-29 | 2019-10-11 | 陈利民 | A kind of beautiful ocular fluid |
| CN110959633A (en) * | 2019-10-29 | 2020-04-07 | 湖北工程学院 | Callicarpa longifolia extract and preparation method and application thereof |
| CN111388405A (en) * | 2020-05-26 | 2020-07-10 | 广州雅纯化妆品制造有限公司 | Oil-control acne-removing composition |
| CN113332192A (en) * | 2021-05-14 | 2021-09-03 | 奈安制药(中国)有限公司 | Callicarpa japonica fruit fermentation product and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105943436A (en) * | 2016-05-29 | 2016-09-21 | 徐国财 | Anti-ultraviolet and anti-aging skin care product and preparation method thereof |
| CN107669531A (en) * | 2016-12-12 | 2018-02-09 | 青岛大学 | A kind of pale spot skin cosmetics |
| CN110314114A (en) * | 2018-03-29 | 2019-10-11 | 陈利民 | A kind of beautiful ocular fluid |
| CN109007439A (en) * | 2018-07-25 | 2018-12-18 | 广州格雷特生物科技有限公司 | Containing callicarpa nudiflora prawn feed additive and its preparation method and application |
| CN109007439B (en) * | 2018-07-25 | 2021-12-14 | 广州格雷特生物科技有限公司 | Prawn feed additive containing callicarpa nudiflora and preparation method and application thereof |
| CN110959633A (en) * | 2019-10-29 | 2020-04-07 | 湖北工程学院 | Callicarpa longifolia extract and preparation method and application thereof |
| CN111388405A (en) * | 2020-05-26 | 2020-07-10 | 广州雅纯化妆品制造有限公司 | Oil-control acne-removing composition |
| CN111388405B (en) * | 2020-05-26 | 2021-08-17 | 广州雅纯化妆品制造有限公司 | Oil-control acne-removing composition |
| CN113332192A (en) * | 2021-05-14 | 2021-09-03 | 奈安制药(中国)有限公司 | Callicarpa japonica fruit fermentation product and preparation method and application thereof |
| CN113332192B (en) * | 2021-05-14 | 2022-10-25 | 奈安制药(中国)有限公司 | Callicarpa japonica fruit fermentation product and preparation method and application thereof |
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