CN107349156A - A kind of plant composition and its preparation method and application - Google Patents
A kind of plant composition and its preparation method and application Download PDFInfo
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- CN107349156A CN107349156A CN201710751483.2A CN201710751483A CN107349156A CN 107349156 A CN107349156 A CN 107349156A CN 201710751483 A CN201710751483 A CN 201710751483A CN 107349156 A CN107349156 A CN 107349156A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/524—Preservatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
Abstract
The invention provides a kind of plant composition and its preparation method and application, the plant composition includes by weight percentage：Grape fruit extract 1 40%, Flos Caryophylli extract 1 40%, Radix Pulsatillae extract 1 40% and common cnidium fruit P.E 1 20%.The plant society composition formula of the present invention is reasonable, Multiple components Synergistic, has antibacterial broad spectrum activity and anti-aging, it is ensured that the stability of cosmetics quality and effect.
Description
Technical field
The invention belongs to cosmetic field, is related to a kind of plant composition and its preparation method and application, and in particular to one
The plant composition of kind with preservative efficacy and its preparation method and application.
Background technology
The organic principles such as the lipid, hydro carbons and the water soluble polymer that are rich in cosmetics, being provided for microorganism growth must
Carbon source, nitrogen source and the energy needed.Under normal temperature environment, the cosmetics easily microbe inoculation behind Kaifeng, cause cosmetics muddy, heavy
The consequence such as shallow lake, foaming, spoiled.Therefore, in order to ensure the quality and effect of cosmetics, it is necessary to add antibacterial and sterilization component to protect
Hold the stability of microorganism in cosmetics.
《Cosmetics health specification》Definition, preservative are to suppress the thing that the growth and breeding of microorganism in cosmetics adds
Matter.Traditional preservatives are mostly artificial preservative, although fungistatic effect is preferable, can cause potential skin irritatin and mistake
Quick reaction.For example, nipagin esters can cause endocrinopathy, KF88 easily causes allergic, and double imidazolidinyl urea contains formaldehyde
Phenomena such as carcinogenic risk, Phenoxyethanol easily causes face heating, shouting pain be present in releaser.Natural antiseptic agent materials are green safe,
But bactericidal effect is little, if being excessively added to obtain good bactericidal effect, the stability of State of cosmetics can be destroyed,
And its toxicity is often higher than synthetic preservative.Therefore, it is necessary to develop a kind of low new toxicity, good antimicrobial effect, have
The compound or composition of preservative efficacy.
The C of CN 1138476 disclose disinfectant and its production method containing Banlangen, the disinfectant bag
20 Chinese medicines such as cloves, climbing groundsel, the Chinese bulbul, chenopodium ambrosiodies, eucalyptus robusta, frutus cnidii, Banlangen are included, to bacterium, fungi, disease
Poison, protozoon, conveyor screw etc. have killing and an inhibitory action, and to skin, mucous membrane it is non-stimulated, without allergic reaction.But this disappears
It is complicated to kill microbial inoculum materials, preparation technology is cumbersome, is added to the stability that State of cosmetics may be destroyed in cosmetics.
The A of CN 102462644 disclose a kind of sterilizing skin-cleansing agent and its production technology, including cloves, climbing groundsel, white
Head father-in-law, chenopodium ambrosiodies, frutus cnidii, the red sage root, Herba portulacae and Chinese violet, have the effect of notable to various skin infections, spot tinea, are
A kind of medicament, it is not suitable as anticorrosive additive and is used in cosmetics.
The A of CN 104904822 disclose a kind of plant source compound antistaling agent for cold fresh meat and preparation method thereof, including
Ginger juice, mint juice, asparagus juice, cloves solution, cassia bark solution, rosemary solution, Tea Polyphenols and grapefruit seed extract, can
Effectively to extend the shelf-life of cold fresh meat, Tea Polyphenols therein has the function that antibacterial and sterilization, grapefruit seed extract tool
There is the effect of antimicrobial spectrum bandwidth, strength is efficient, but can not still be applied to cosmetic field.
Therefore it provides a kind of composition with antisepsis using natural plants as primary raw material, suppresses in cosmetics
The growth and breeding of microorganism, it is ensured that the stability of cosmetics quality and effect, have great importance in cosmetic field and
Wide market prospects.
The content of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of plant composition and its preparation method and application, institute
Plant composition is stated using natural plants as primary raw material, sterilizing ability is strong, antibacterial broad spectrum activity is good, can be effective for cosmetics series
Suppress the growth of microorganism, prepare the cosmetics that property is stable, antiseptic effect is good.
In a first aspect, the invention provides a kind of plant composition, it is characterised in that the plant composition by weight hundred
Ratio is divided to include：Grape fruit extract 1-40%, Flos Caryophylli extract 1-40%, Radix Pulsatillae extract 1-40% and common cnidium fruit P.E
1-20%.
The effect of each plant extracts, is as follows：
Grape fruit extract is a kind of antibacterial material of strong effect wide-spectrum, to staphylococcus aureus, Escherichia coli and typhoid fever
The bacteriums such as bacillus are respectively provided with higher bacteriostatic activity；Meanwhile grape fruit also has trophocyte, inducing diuresis to remove edema, pore refining
Effect, available for conditioning and deep layer purification mixed type, oily skin, there is desalination dark sore, congested skin of releiving, promote hair life
The effect of long and Rosemary Extract.
Flos Caryophylli extract is to staphylococcus aureus, Escherichia coli, production acidfast bacilli, bacillus sulph-hydrogenus and bacillus cloacae etc.
Bacterium and a variety of fungies have stronger suppression and killing action, have and stimulate circulation, treat skin ulcer and wound hair
Scorching, treatment mange, the effect for improving coarse skin.
Radix Pulsatillae extract contains the composition such as Herba Ranunculi Japonici glycoside protoanemonin and triterpene saponin pulchinenoside, and its is effective
Antimicrobial component is protoanemonin and Anemonin, can suppress golden yellow grape bacillus, Pseudomonas aeruginosa, Escherichia coli and secondary wound
The growth and breeding of the microorganisms such as cold bacillus.
Osthole in common cnidium fruit P.E has strong suppression to fungies such as Alternariaspp, Cryptococcus neoformans and Aspergillus
Make and use, for treating anaphylactia, treatment skin disease, the key medicine of pruritus are considered as by ancient Chinese medicine doctor.
Plant composition provided by the invention is using grape fruit extract, Flos Caryophylli extract and Radix Pulsatillae extract as main group
Point, coordinate jointly with common cnidium fruit P.E, act synergistically, can effectively suppress staphylococcus aureus, Escherichia coli, green pus bar
The growth of bacterium, Candida albicans and aspergillus niger, fungistatic effect are notable.
Preferably, the percentage by weight of the grape fruit extract is 1-40%, for example, can be 1%, 2%, 5%,
8%th, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 28%, 30%, 32%, 35%, 38% or 40%, be preferably
30-40%, more preferably 30%.
Preferably, the percentage by weight of the Flos Caryophylli extract is 1-40%, for example, can be 1%, 2%, 5%, 8%,
10%th, 12%, 15%, 18%, 20%, 22%, 25%, 28%, 30%, 32%, 35%, 38% or 40%, preferably 10-
25%, more preferably 25%.
Preferably, the percentage by weight of the Radix Pulsatillae extract is 1-40%, for example, can be 1%, 2%, 5%,
8%th, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 28%, 30%, 32%, 35%, 38% or 40%, be preferably
25-35%, more preferably 30%.
Preferably, the percentage by weight of the common cnidium fruit P.E is 1-20%, for example, can be 1%, 2%, 3%,
4%th, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or
20%, preferably 10-15%, more preferably 15%.
Preferably, the plant composition includes by weight percentage：Grape fruit extract 30-40%, Flos Caryophylli extract
10-25%, Radix Pulsatillae extract 25-35% and common cnidium fruit P.E 10-15%.
Preferably, the plant composition includes by weight percentage：Grape fruit extract 30%, Flos Caryophylli extract
25%th, Radix Pulsatillae extract 30% and common cnidium fruit P.E 15%.
Second aspect, the invention provides a kind of method for preparing plant composition as described in relation to the first aspect, including such as
Lower step：
(1) pre-process：Plant composition each component raw material is crushed, sieving；
(2) homogeneous extracts：Plant granule after crushing is placed in high pressure homogenizer, after adding Extraction solvent immersion, entered
Horizontal high voltage homogeneous extracts；
(3) purifying elution：Extract solution is centrifuged, purified, eluted, obtains eluent；
(4) concentration mixing：Eluent is concentrated under reduced pressure, the plant society is prepared after being mixed according to formula
Thing.
Preferably, the mesh number of step (1) described sieving is 80-120 mesh, for example, can be 80 mesh, 85 mesh, 90 mesh, 95 mesh,
100 mesh, 105 mesh, 110 mesh, 115 mesh or 120 mesh, preferably 100 mesh.
Preferably, the feed liquid mass ratio of step (2) plant granule and the Extraction solvent is 1:(5-30), such as can
To be 1:5、1:6、1:7、1:8、1:9、1:10、1:11、1:12、1:13、1:14、1:15、1:16、1:17、1:18、1:19、1:
20、1:21、1:22、1:23、1:24、1:25、1:26、1:27、1:28、1:29 or 1:30, preferably 1:(10-15).
Preferably, step (2) described Extraction solvent includes any one in water, ethanol or butanediol or at least two
Combination, the preferably combination of water and ethanol.
Preferably, the mass fraction of the ethanol is 30-95%, for example, can be 30%, 35%, 40%, 45%,
50%th, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% or 95%, preferably 50-80%, more preferably
60%.
Preferably, the time of step (2) described immersion is 1-2h, for example, can be 1h, 1.1h, 1.2h, 1.3h, 1.4h,
1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2h.
Preferably, step (2) the high-pressure homogeneous extraction time is 20-40min, for example, can be 20min, 21min,
22min、23min、24min、25min、26min、27min、28min、29min、30min、31min、32min、33min、
34min, 35min, 36min, 37min, 38min, 39min or 40min, preferably 25-30min.
Preferably, step (2) the high-pressure homogeneous extraction pressure is 50-120MPa, for example, can be 50MPa,
55MPa、60MPa、65MPa、70MPa、75MPa、80MPa、85MPa、90MPa、95MPa、100MPa、105MPa、110MPa、
115MPa or 120MPa, preferably 80-100MPa.
Preferably, step (3) purifying is purified using macroporous resin column.
Preferably, the large aperture resin is D101 and/or AB-8 resin columns.
Preferably, step (3) elution is carried out using any one in ethanol, water or butanediol or at least two combination
Elution.
Preferably, the mass fraction of the ethanol is 10-95%, for example, can be 10%, 15%, 20%, 25%,
30%th, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% or 95%, be preferably
50-80%, more preferably 60%.
Preferably, step (4) pressure being concentrated under reduced pressure is -0.07~-0.1MPa, for example, can be -0.07MPa, -
0.08MPa, -0.09MPa, -0.1MPa, it is preferably -0.08MPa.
In the present invention, the processing mode of each raw material of plant composition can be independently selected from above-mentioned condition, mutual not shadow
Ring.
The third aspect, it is used to prepare cosmetics the invention provides a kind of plant composition as described in relation to the first aspect.
Preferably, the addition of the plant composition is 2-20%, for example, can be 2.0%, 2.5%, 3.0%,
3.5%th, 4.0%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%,
9.5%th, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15%,
15.5%th, 16%, 16.5%, 17%, 17.5%, 18%, 18.5%, 19%, 19.5% or 20%, preferably 5-15%.
Preferably, the formulation of the cosmetics includes：It is any in aqua, emulsion, spray, cream, elite or facial mask
It is a kind of or at least two combination, preferably emulsion and/or cream agent.
Compared with prior art, the present invention has the advantages that：
(1) bacteriostasis property is excellent：To staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Candida albicans and aspergillus niger
Obvious killing action is respectively provided with, 23.15mm is up to the antibacterial circle diameter of bacterium, the antibacterial circle diameter of fungi is up to
21.67mm；
(2) anti-aging performance is notable：60% is more than to the clearance rate of ultra-oxygen anion free radical, the removing to hydroxy radical
Rate is more than 70%；
(3) it is nonirritant：L/D values are equal>100, in nonirritant；
(4) skin care item of the plant composition prepared added with the present invention have the ability for suppressing growth of microorganism breeding,
Good antiseptic property is showed, and does not have excitant and sensitization to skin.
Embodiment
For the present invention technological means and its effect taken is expanded on further, the present invention is made with reference to embodiments into
Illustrate to one step.It is understood that embodiment described herein is used only for explaining the present invention, rather than to this hair
Bright restriction.
In the examples where no specific technique or condition is specified, according to the technology or condition described by document in the art,
Or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, be can be by regular channel commercially available from
The conventional products of acquisition.
The preparation of the plant composition of embodiment 1 (I)
Grapefruit peel is crushed, 100 mesh sieves is crossed, is placed in high pressure homogenizer, is 1 by solid-liquid ratio:10 add 60% ethanol
The aqueous solution, after soaking 1.5h, high pressure homogenization method 30min, extraction pressure is 80MPa, after extract solution is centrifuged, upper D101
Large aperture resin is purified, and is eluted with 60% ethanol water, collect eluent carry out depressurizing under -0.08MPa it is dense
Contracting, obtains medicinal extract shape grape fruit extract.
Lilac is crushed, 100 mesh sieves is crossed, is placed in high pressure homogenizer, is 1 by solid-liquid ratio:15 add butanediol, immersion
After 1.5h, high pressure homogenization method 25min, extraction pressure is 100MPa, after extract solution is centrifuged, upper D101 large apertures resin
Purified, eluted with butanediol, collected eluent and be concentrated under reduced pressure under -0.08MPa, obtain medicinal extract shape cloves and carry
Take thing.
The Chinese bulbul is crushed, 100 mesh sieves is crossed, is placed in high pressure homogenizer, is 1 by solid-liquid ratio:15 add butanediol, immersion
After 1.5h, high pressure homogenization method 25min, extraction pressure is 100MPa, after extract solution is centrifuged, upper D101 large apertures resin
Purified, eluted with butanediol, collected eluent and be concentrated under reduced pressure under -0.08MPa, obtain the medicinal extract shape Chinese bulbul
Extract.
Frutus cnidii is crushed, 100 mesh sieves is crossed, is placed in high pressure homogenizer, is 1 by solid-liquid ratio:10 add 70% ethanol water
Solution, after soaking 1.5h, high pressure homogenization method 30min, extraction pressure is 80MPa, and after extract solution is centrifuged, upper D101 is big
Aperture resin is purified, and is eluted with 70% ethanol water, is collected eluent and is concentrated under reduced pressure under -0.08MPa,
Obtain medicinal extract shape common cnidium fruit P.E.
By Four Plants extract according to 30% grape fruit extract, 25% Flos Caryophylli extract, 30% Radix Pulsatillae extract
With 15% common cnidium fruit P.E, configuration obtains plant composition (I).
The preparation of the plant composition of embodiment 2 (II)
Grapefruit peel, lilac, the Chinese bulbul and frutus cnidii Four Plants raw material are crushed respectively, 105 mesh sieves is crossed, is placed in height
Press in homogenizer, be 1 by solid-liquid ratio:10 add 50% ethanol water, after soaking 1.4h, high pressure homogenization method 25min, and extraction
Pressure is 80MPa, and after extract solution is centrifuged, upper AB-8 large apertures resin is purified, and is carried out with 50% ethanol water
Elution, collect eluent and be concentrated under reduced pressure under -0.08MPa, obtain medicinal extract shape plant extracts.
By Four Plants extract according to 35% grape fruit extract, 10% Flos Caryophylli extract, 35% Radix Pulsatillae extract
With 20% common cnidium fruit P.E, configuration obtains plant composition (II).
The preparation of the plant composition of embodiment 3 (III)
Grapefruit peel, lilac, the Chinese bulbul and frutus cnidii Four Plants raw material are crushed respectively, 95 mesh sieves is crossed, is placed in height
Press in homogenizer, be 1 by solid-liquid ratio:15 add 80% ethanol water, after soaking 1.6h, high pressure homogenization method 30min, and extraction
Pressure is 100MPa, and after extract solution is centrifuged, upper D101 large apertures resin is purified, and is carried out with 80% ethanol water
Elution, collect eluent and be concentrated under reduced pressure under -0.08MPa, obtain medicinal extract shape plant extracts.
By Four Plants extract according to 40% grape fruit extract, 25% Flos Caryophylli extract, 25% Radix Pulsatillae extract
With 10% common cnidium fruit P.E, configuration obtains plant composition (III).
The preparation of the plant composition of embodiment 4 (IV)
Grapefruit peel, lilac, the Chinese bulbul and frutus cnidii Four Plants raw material are crushed respectively, 110 mesh sieves is crossed, is placed in height
Press in homogenizer, be 1 by solid-liquid ratio:8 add 30% ethanol water, after soaking 1.2h, high pressure homogenization method 22min, and extraction
Pressure is 65MPa, and after extract solution is centrifuged, upper AB-8 large apertures resin is purified, and is carried out with 30% ethanol water
Elution, collect eluent and be concentrated under reduced pressure under -0.08MPa, obtain medicinal extract shape plant extracts.
By Four Plants extract according to 1% grape fruit extract, 40% Flos Caryophylli extract, 40% Radix Pulsatillae extract and
19% common cnidium fruit P.E, configuration obtain plant composition (IV).
The preparation of the plant composition of embodiment 5 (V)
Grapefruit peel, lilac, the Chinese bulbul and frutus cnidii Four Plants raw material are crushed respectively, 90 mesh sieves is crossed, is placed in height
Press in homogenizer, be 1 by solid-liquid ratio:20 add 95% ethanol water, after soaking 1.8h, high pressure homogenization method 35min, and extraction
Pressure is 110MPa, and after extract solution is centrifuged, upper D101 large apertures resin is purified, and is carried out with 95% ethanol water
Elution, collect eluent and be concentrated under reduced pressure under -0.07MPa, obtain medicinal extract shape plant extracts.
By Four Plants extract according to 39% grape fruit extract, 1% Flos Caryophylli extract, 40% Radix Pulsatillae extract and
20% common cnidium fruit P.E, configuration obtain plant composition (V).
The preparation of the plant composition of embodiment 6 (VI)
Grapefruit peel, lilac, the Chinese bulbul and frutus cnidii Four Plants raw material are crushed respectively, 120 mesh sieves is crossed, is placed in height
Press in homogenizer, be 1 by solid-liquid ratio:5 add deionized water, and after soaking 1h, high pressure homogenization method 20min, extracting pressure is
50MPa, after extract solution is centrifuged, upper AB-8 large apertures resin is purified, and is eluted with 10% ethanol water, is received
Collection eluent is concentrated under reduced pressure under -0.09MPa, obtains medicinal extract shape plant extracts.
By Four Plants extract according to 40% grape fruit extract, 39% Flos Caryophylli extract, 1% Radix Pulsatillae extract and
20% common cnidium fruit P.E, configuration obtain plant composition (VI).
The preparation of the plant composition of embodiment 7 (VII)
Grapefruit peel, lilac, the Chinese bulbul and frutus cnidii Four Plants raw material are crushed respectively, 80 mesh sieves is crossed, is placed in height
Press in homogenizer, be 1 by solid-liquid ratio:30 add butanediol, and after soaking 2h, high pressure homogenization method 40min, extracting pressure is
120MPa, after extract solution is centrifuged, upper D101 large apertures resin is purified, and is eluted with butanediol, collects elution
Liquid is concentrated under reduced pressure under -0.1MPa, obtains medicinal extract shape plant extracts.
By Four Plants extract according to 40% grape fruit extract, 40% Flos Caryophylli extract, 19% Radix Pulsatillae extract
With 1% common cnidium fruit P.E, configuration obtains plant composition (VII).
Comparative example 1
Compared with Example 1, plant composition includes 45% grape fruit extract, 45% Flos Caryophylli extract, 0.5% hoary hair
Father-in-law's extract and 9.5% common cnidium fruit P.E, other preparation process are same as Example 1.
Comparative example 2
Compared with Example 1, plant composition includes 9.5% grape fruit extract, 45% Flos Caryophylli extract, 45% hoary hair
Father-in-law's extract and 0.5% common cnidium fruit P.E, other preparation process are same as Example 1.
Comparative example 3
Compared with Example 1, plant composition includes 0.5% grape fruit extract, 29.5% Flos Caryophylli extract, 45% white
Head father-in-law's extract and 25% common cnidium fruit P.E, other preparation process are same as Example 1.
Comparative example 4
Compared with Example 1, plant composition includes 45% grape fruit extract, 0.5% Flos Caryophylli extract, 29.5% white
Head father-in-law's extract and 25% common cnidium fruit P.E, other preparation process are same as Example 1.
Comparative example 5
Compared with Example 1, in addition to not containing grape fruit extract, plant composition extracts including 40% cloves
Thing, 40% Radix Pulsatillae extract and 20% common cnidium fruit P.E, other preparation process are same as Example 1.
Comparative example 6
Compared with Example 1, in addition to not containing Flos Caryophylli extract, plant composition extracts including 40% grape fruit
Thing, 40% Radix Pulsatillae extract and 20% common cnidium fruit P.E, other preparation process are same as Example 1.
Comparative example 7
Compared with Example 1, in addition to not containing Radix Pulsatillae extract, plant composition extracts including 40% grape fruit
Thing, 40% Flos Caryophylli extract and 20% common cnidium fruit P.E, other preparation process are same as Example 1.
Comparative example 8
Compared with Example 1, in addition to not containing common cnidium fruit P.E, plant composition extracts including 35% grape fruit
Thing, 35% Flos Caryophylli extract and 30% Radix Pulsatillae extract, other preparation process are same as Example 1.
Comparative example 9
Plant composition only includes 100% grape fruit extract.
Comparative example 10
Plant composition only includes 100% Flos Caryophylli extract.
Comparative example 11
Plant composition only includes 100% Radix Pulsatillae extract.
Comparative example 12
Plant composition only includes 100% common cnidium fruit P.E.
Inhibition zone instruction experiment
Comprise the following steps that：
(1) actication of culture：Under aseptic condition, the culture medium of sterilizing is loaded in test tube and forms inclined-plane, is moved with method of scoring
Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Candida albicans and aspergillus niger are connect, is put into incubator, bacterium is in 37 DEG C
Lower culture 24h, fungi are cultivated 3-5 days at 28 DEG C；
(2) preparation of bacterium suspension is indicated：Under aseptic condition, the thalline that has been activated with the ring of oese picking 2 uses physiology salt
Water is diluted, and concussion mixes, and the concentration of each strain is controlled 105-106cfu/mL；
(3) Odontothrips loti inhibition zone instruction experiment：Under aseptic condition, draw 200 μ L indicator bacteria uniform suspensions and be coated on
On plating medium, each culture medium moderate distance steadily places 6 sterile Oxford cups；Be added dropwise respectively to Oxford cup 0.25mL by
The concentration that embodiment 1-7 and comparative example 1-8 plant composition configures is 0.1g/mL sample solution, wherein, indicator bacteria is gold
Staphylococcus aureus, Escherichia coli and the culture of Pseudomonas aeruginosa are based on 37 DEG C of culture 24h, and indicator bacteria is Candida albicans and black song
Mould culture is based on 28 DEG C and cultivated 3-5 days；Oxford cup is removed, with the diameter of each inhibition zone of slide measure accurate measuring, compares suppression
Bacterium effect.
Experimental result is as shown in table 1.
The instruction experiment of the inhibition zone of table 1
Contrasted from embodiment 1-7, when plant composition includes grape fruit extract 30%, Flos Caryophylli extract 25%, white
When head father-in-law extract 30% and common cnidium fruit P.E 15%, there is most strong fungistatic effect, show obvious cooperative effect, it is right
Bacterium and fungi show good bacteriostasis, wherein, 23.15mm is up to the antibacterial circle diameter of bacterium, to fungi
Antibacterial circle diameter be up to 21.67mm.
In the case of preparation technology identical, compared with Example 1, the weight percent of comparative example 1-4 plant extracts
Than outside the scope of protection of present invention, bacteriostasis substantially weakens, the antibacterial circle diameter of bacterium is up to
13.73mm, 14.17mm is up to fungi antibacterial circle diameter；Comparative example 5-8 lacks a Plant Extracts, and bacteriostasis has
Weakened, 11.81mm is up to the antibacterial circle diameter of bacterium, 12.60mm is up to the antibacterial circle diameter of fungi；Comparative example
The 9-12 only plant extracts containing one-component, bacteriostasis significantly reduce, and the antibacterial circle diameter maximum to bacterium is only
7.71mm, to the maximum only 8.53mm of antibacterial circle diameter of fungi.
Anti-senescence function is tested
(1) ultra-oxygen anion free radical Scavenging activity is evaluated
The Tris-HCl buffer solutions (pH=8.2) that 4.5mL concentration is 0.05mol/L are preheated in 25 DEG C of water-baths
20min, the sample solution that the concentration that 1mL is configured by embodiment 1-7 and comparative example 1-8 plant composition is 1% is then added,
The pyrogallol solution that 0.4mL concentration is 25mmol/L is added, mixes after reacting 5min in 25 DEG C of water-baths, adds 1.0mL
Concentration is 8mol/L HCl terminating reactions.Reference is made with Tris-HCl buffer solutions, determines the absorbance at 299nm.Blank pair
Solvent according to group for isometric sample.Evaluation of the sample to ultra-oxygen anion free radical Scavenging activity is calculated with following formula, in formula
A1 is the absorbance of blank control, and A2 is the absorbance of sample.
Ultra-oxygen anion free radical clearance rate (%)=[1- (A2/A1)] × 100%
(2) to Hydroxyl radical-scavenging merit rating
The FeSO that 3mL concentration is 2mmol/L is sequentially added in 25mL colorimetric cylinders4, 3mL concentration is 1mmol/L H2O2,
3mL concentration is 6mmol/L salicylic acid, shakes up after 37 DEG C of heating water bath 15min, determines absorbance；It is separately added into by reality
The sample solution that a 1-7 and comparative example 1-8 plant composition configures is applied, rear heating water bath 15min is shaken up, determines absorbance
Value.Blank control group is the solvent of isometric sample.Evaluation of the sample to Hydroxyl radical-scavenging ability is calculated with following formula, in formula
A1 is the absorbance of reaction system before sample-adding product, and A2 is the absorbance of reaction system after sample scavenging hydroxyl, and A3 is
The absorbance of reaction system after blank control scavenging hydroxyl.
Scavenging action to hydroxyl free radical (%)=[A1-A2- (A1-A3)]/A1 × 100%
Experimental result is as shown in table 2.
The anti-senescence function of table 2 is tested
| Numbering | Ultra-oxygen anion free radical clearance rate (%) | Scavenging action to hydroxyl free radical (%) |
| Embodiment 1 | 68.38 | 76.64 |
| Embodiment 2 | 67.47 | 75.43 |
| Embodiment 3 | 66.58 | 75.26 |
| Embodiment 4 | 64.95 | 74.30 |
| Embodiment 5 | 64.17 | 73.65 |
| Embodiment 6 | 63.44 | 72.09 |
| Embodiment 7 | 62.22 | 71.16 |
| Comparative example 1 | 59.06 | 69.99 |
| Comparative example 2 | 58.47 | 69.35 |
| Comparative example 3 | 57.95 | 68.10 |
| Comparative example 4 | 57.03 | 66.47 |
| Comparative example 5 | 36.41 | 35.10 |
| Comparative example 6 | 35.51 | 32.07 |
| Comparative example 7 | 32.63 | 31.03 |
| Comparative example 8 | 31.19 | 30.82 |
| Comparative example 9 | 15.76 | 16.42 |
| Comparative example 10 | 12.32 | 13.54 |
| Comparative example 11 | 11.26 | 12.86 |
| Comparative example 12 | 10.11 | 11.65 |
Embodiment 1-7 plant composition has stronger anti-aging ability, to the clearance rate of ultra-oxygen anion free radical
More than 60%, 70% is more than to the clearance rate of hydroxy radical, wherein, when plant composition includes grape fruit extract 30%, fourth
When fragrant extract 25%, Radix Pulsatillae extract 30% and common cnidium fruit P.E 15%, there is most strong anti-aging ability, show
Obvious cooperative effect, good Scavenging activity is respectively provided with to superoxide anion and hydroxy radical, wherein, superoxide anion is free
Base clearance rate is up to 68.38%, and Scavenging action to hydroxyl free radical is up to 76.64%.
In the case of preparation technology identical, compared with Example 1, the weight percent of comparative example 1-4 plant extracts
Than outside the scope of protection of present invention, radical scavenging activity substantially weakens；Comparative example 5-8 lacks a kind of plant extract
Thing, radical scavenging activity have weakened；The comparative example 9-12 only plant extracts containing one-component, radical scavenging activity
Significantly reduce, ultra-oxygen anion free radical clearance rate highest only 15.76%, Scavenging action to hydroxyl free radical highest only 16.42%.
Erythrocyte hemolysis is tested
Erythrocyte hemolysis experiment is lagophthalmos stimulation test (Draize test) alternative, and general principle is to pass through survey
Determine hemoglobin stripping quantity and denaturation degrees carry out damage of the evaluating chemical product to ocular tissue's cell.Mainly pass through red blood cell in the world
Hemolytic experiment evaluates the excitant of cosmetics and its raw material to eye.
The plant composition that this experiment prepares embodiment 1-7 carries out erythrocyte hemolysis experiment, and according to European alternative
The method of testing and grade scale (ECVAM.ECVAM DB-ALM of the erythrocyte hemolysis experiment of method authentication center (ECVAM):
INVITOX Protocol,Red blood cells test system.INVITOX No.37.Ispra.Italy:ECVAM,
1994) excitant of plant composition is evaluated.Table 3 is ECVAM to the irritating grade scale of cosmetics.
The table 3ECVAM irritating grade scale of cosmetics
Table 4 is the erythrocyte hemolysis experimental result of each sample.
The erythrocyte hemolysis experimental result of each sample of table 4
| Numbering | L/D | Evaluation |
| Embodiment 1 | 773.82 | It is nonirritant |
| Embodiment 2 | 751.52 | It is nonirritant |
| Embodiment 3 | 737.21 | It is nonirritant |
| Embodiment 4 | 722.80 | It is nonirritant |
| Embodiment 5 | 654.59 | It is nonirritant |
| Embodiment 6 | 645.92 | It is nonirritant |
| Embodiment 7 | 636.57 | It is nonirritant |
As can be seen from Table 4, embodiment 1-7 L/D values are equal>100, illustrate plant composition in nonirritant.Therefore, should
Plant composition is safe, non-stimulated to skin, belongs to natural, non-stimulated raw material, can trust addition in cosmetics.
Embodiment 8
Table 5 show the emulsion formulations containing plant composition (I).
The emulsion formulations of table 5
Preparation method is as follows：
(1) aqueous phase material is put into aqueous phase to prepare in pot, heating stirring is to 80-85 DEG C；
(2) oil phase material is put into oil phase to prepare in pot, heating stirring is to 80-85 DEG C；
(3) material in aqueous phase pot is pumped into emulsification pot, the material in oil phase pot is pumped into emulsification pot, stirring
Emulsification pot is evacuated after uniformly, emulsifying 10 minutes；
(4) 20 minutes are incubated, then using cooling water temperature to 30-35 DEG C；
(5) addition phase is added, stirs, discharges after the assay was approved.
Embodiment 9
Table 6 show the creams formula containing plant composition (I).
The creams formula of table 6
Preparation method is as follows：
(1) aqueous phase material is put into aqueous phase to prepare in pot, heating stirring is to 80-85 DEG C；
(2) oil phase material is put into oil phase to prepare in pot, heating stirring is to 80-85 DEG C；
(3) material in aqueous phase pot is pumped into emulsification pot, the material in oil phase pot is pumped into emulsification pot, stirring
Emulsification pot is evacuated after uniformly, emulsifying 10 minutes；
(4) 20 minutes are incubated, then using cooling water temperature to 30-35 DEG C；
(5) addition phase is added, stirs, discharges after the assay was approved.
Embodiment 10
Compared with Example 8, the addition of plant composition is 2%, and other conditions are same as Example 8.
Embodiment 11
Compared with Example 9, the addition of plant composition is 20%, and other conditions are same as Example 9.
Comparative example 13
Compared with Example 8, the addition of plant composition is 1%, and other conditions are same as Example 8.
Comparative example 14
Compared with Example 9, the addition of plant composition is 25%, and other conditions are same as Example 9.
Microbial Challenge is tested
This laboratory reference U.S. cosmetics toilet articles and essence association (CTFA) standard, are added a certain amount of in cosmetics
Microbial bacteria suspension, in 28 days at regular intervals with colony counting method detect microorganism survival condition, judge preservative
Antiseptic effect.Comprise the following steps that：
20g embodiments 8-11 and comparative example 13-14 each 2 parts of sample is weighed, is placed in aseptic plastic bottle, is separately added into suitable
The bacterial suspension of amount and fungal spore suspension so that the content of bacterium is 1.0 × 10 in sample6-9.0×106Cfu/g, fungi ferment
The content of female bacterium is 1.0 × 105-9.0×105cfu/g.Sample is placed under (28 ± 1) DEG C environment, inoculation the 7th day, 14 days,
Sampled after 21 days and 28 days, according to the bacteria containing amount in flat board tilt-pour process count samples.
The bacterial content reduction by 99.9% at the 7th day of preservation challenge requirement of experiment, fungal content reduction by 90%, and
14th, continuous decrease (N.I=no increase) in 21 and 28 days, specific criterion is as shown in table 7.
The preservation challenge criterion of table 7
Microbial Challenge experimental result is as shown in table 8-9.
The Bacterial challenges of table 8 are tested
The Fungal challenges of table 9 are tested
Microbial Challenge test result indicates that, the cosmetics of the plant composition added with 2%-20% can pass through challenge
Experiment, bacterial content reduces 99.999% at the 7th day, and fungal content reduces 99.99%, and is held in 14,21,28 days
It is continuous to decline, there is good preservative efficacy.
In comparative example 13, the addition of plant composition is 1%, can not effectively play the work suppressed growth of microorganism
With；In comparative example 14, the addition of plant composition is 25.0%, although with very strong antiseptic property, addition
The excessive stability for destroying State of cosmetics.
In summary, plant composition (1) bacteriostasis property that prepared by the present invention is excellent：To staphylococcus aureus, large intestine
Bacillus, Pseudomonas aeruginosa, Candida albicans and aspergillus niger are respectively provided with obvious killing action, and the antibacterial circle diameter of bacterium is up to
23.15mm, 21.67mm is up to the antibacterial circle diameter of fungi；(2) anti-aging performance is notable：To ultra-oxygen anion free radical
Clearance rate be more than 60%, 70% is more than to the clearance rate of hydroxy radical；(3) it is nonirritant：L/D values are equal>100, in non-stimulated
Property；(4) skin care item of the plant composition prepared added with the present invention have the function that to suppress growth of microorganism, and show good
Antiseptic property, and do not have excitant and sensitization to skin.
Applicant states that the present invention illustrates the method detailed of the present invention, but not office of the invention by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (10)
1. a kind of plant composition, it is characterised in that the plant composition includes by weight percentage：Grape fruit extract 1-
40%th, Flos Caryophylli extract 1-40%, Radix Pulsatillae extract 1-40% and common cnidium fruit P.E 1-20%.
2. plant composition according to claim 1, it is characterised in that the plant composition wraps by weight percentage
Include：Grape fruit extract 30-40%, Flos Caryophylli extract 10-25%, Radix Pulsatillae extract 25-35% and common cnidium fruit P.E 10-
15%.
3. plant composition according to claim 1 or 2, it is characterised in that the plant composition is by weight percentage
Including：Grape fruit extract 30%, Flos Caryophylli extract 25%, Radix Pulsatillae extract 30% and common cnidium fruit P.E 15%.
A kind of 4. method for preparing the plant composition as any one of claim 1-3, it is characterised in that including following step
Suddenly：
(1) pre-process：Plant composition each component raw material is crushed, sieving；
(2) homogeneous extracts：Plant granule after crushing is placed in high pressure homogenizer, after adding Extraction solvent immersion, carried out high
Press homogeneous extraction；
(3) purifying elution：Extract solution is centrifuged, purified, eluted, obtains eluent；
(4) concentration mixing：Eluent is concentrated under reduced pressure, the plant composition is prepared after being mixed according to formula.
5. according to the method for claim 4, it is characterised in that the mesh number of step (1) described sieving is 80-120 mesh, preferably
For 100 mesh.
6. the method according to claim 4 or 5, it is characterised in that step (2) plant granule and the Extraction solvent
Feed liquid mass ratio be 1:(5-30), preferably 1:(10-15)；
Preferably, group of step (2) the described Extraction solvent including any one in water, ethanol or butanediol or at least two
Close, the preferably combination of water and ethanol；
Preferably, the mass fraction of the ethanol is 30-95%, preferably 50-80%, more preferably 60%；
Preferably, the time of step (2) described immersion is 1-2h；
Preferably, step (2) the high-pressure homogeneous extraction time is 20-40min, preferably 25-30min；
Preferably, step (2) the high-pressure homogeneous extraction pressure is 50-120MPa, preferably 80-100MPa.
7. according to the method described in claim any one of 4-6, it is characterised in that step (3) purifying uses macroreticular resin
Post is purified；
Preferably, the large aperture resin is D101 and/or AB-8 resin columns；
Preferably, step (3) elution is washed using any one in ethanol, water or butanediol or at least two combination
It is de-；
Preferably, the mass fraction of the ethanol is 10-95%, preferably 50-80%, more preferably 60%.
8. according to the method described in claim any one of 4-7, it is characterised in that step (4) pressure being concentrated under reduced pressure for-
0.07~-0.1MPa, it is preferably -0.08MPa.
9. a kind of plant composition as any one of claim 1-3 is used to prepare cosmetics；
Preferably, the addition of the plant composition is 2-20%, preferably 5-15%.
10. cosmetics according to claim 9, it is characterised in that the formulation of the cosmetics includes：Aqua, emulsion, spray
In mist agent, cream, elite or facial mask any one or at least two combination, preferably emulsion and/or cream agent.
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| CN114886813A (en) * | 2022-05-27 | 2022-08-12 | 广州环亚化妆品科技股份有限公司 | Anti-aging plant extract composition and preparation method and application thereof |
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