CN108113924A

CN108113924A - A kind of composite plant Shu Min agent and preparation method and application

Info

Publication number: CN108113924A
Application number: CN201711441736.2A
Authority: CN
Inventors: 晏洁; 麦康; 丘北泳; 肖少宇; 谢培镇; 陈杰烽; 郑华生; 黄桂州; 张鹏; 程建华
Original assignee: ZHONGSHAN AIHU COMMODITY CO Ltd; Guangzhou Chao Hui Biological Technology Co Ltd
Current assignee: ZHONGSHAN AIHU COMMODITY CO Ltd; Guangzhou Chao Hui Biological Technology Co Ltd
Priority date: 2017-12-27
Filing date: 2017-12-27
Publication date: 2018-06-05

Abstract

The invention discloses a kind of composite plant Shu Min agent and preparation method and application.Wild chrysanthemum flavones and preservative are dispersed with stirring in polyalcohol by the present invention, at a certain temperature homogeneous, obtain mixture I；Forsythia volatile oil, grease and emulsifier are mixed and are uniformly dispersed, obtains mixtures II；Honegsukle flower P.E and water are mixed and are uniformly dispersed, obtains mixtures III；Mixture I and mixtures III are sufficiently mixed, mixtures II is added under certain mixing speed, homogeneous obtains composite plant Shu Min agent.Different deliquescent plant functional components are combined with each other by the present invention by microemulsion technology, are added lipophilicity and the dissolubility of hydrophily Shu Min ingredients, can be played Shu Min effects at many levels from water phase, oil phase, Shu Min effects are good, are suitable for preparing cosmetics.

Description

A kind of composite plant Shu Min agent and preparation method and application

Technical field

The invention belongs to cosmetic technical field, more particularly to a kind of composite plant Shu Min agent and preparation method thereof is with answering With.

Background technology

With a large amount of uses of cosmetics, skin disease also rolls up caused by cosmetics.Cosmetics by emulsifier, Into being grouped into, these ingredients are to synthesize to obtain by chemical mode mostly, right for moisturizer, thickener, essence, pigment, preservative etc. Application on human skin has sensitization risk.If emulsifier can destroy skin texture, cause skin sensitivity；Pigment easily causes pigment and sinks It, triggers color spot；Fragrance has strong sensitization, easily triggers allergic reaction；Preservative has also killed while harmful bacteria is killed Beneficial bacteria reduces defencive function of skin itself etc..It can be easy to cause allergic phenomena with inappropriate cosmetics.

Skin allergy is a kind of stress reaction after skin contact anaphylactogen, and after skin contact anaphylactogen, human body can produce Raw Anaphylactic mediator, Anaphylactic mediator serve directly, generate a series of phenomena of cutaneous irritation.Common skin allergy medium has group Amine (HIS), interleukin 1 (IL-1), interleukin-6 (IL-6), tumor necrosis factor (TNF-a), serotonin (5- HT), leukotriene B4 (LTB4) etc..

At present, common cosmetics antiallergic ingredient has：Bisabolol, dipotassium glycyrrhizinate, aloe extract, chamomile extraction Object etc..Bisabolol eliminates erythema by inhibiting inflammatory mediator interleukins (IL-1), leukotriene B4 (LTB4)；Glycyrrhizic acid Dipotassium is by preventing the release of histamine, removing toxic substances disinfection, antiallergy；Aloe extract has anti-inflammation and sterilization effect, to bacterium infection Allergy pass through the calm effect antiallergic releived；Chamomile has Shu Min, maintenance sensitivity skin, reduces thin red blood silk, reduces hair It is red, adjustment the colour of skin it is uneven the effects that.

Common antiallergic ingredient usually has the shortcomings of dissolubility is bad, active matter easy in inactivation, Shu Min effects are slow, wherein There are some illegal businessmans to be rapidly achieved only quick effect, the hormones constituents such as some sugared cortex can be added in the product, for a long time Using skin can be caused to generate dependence, once change is stopped using to be easy to recur, go down finally makes skin more sensitive for a long time.

The content of the invention

The shortcomings that primary and foremost purpose of the present invention is to overcome the prior art and deficiency, provide a kind of composite plant Shu Min agent Preparation method.

Another object of the present invention is to provide the composite plant Shu Min agent obtained by above-mentioned preparation method.

It is still another object of the present invention to provide the applications of the composite plant Shu Min agent.

The purpose of the present invention is achieved through the following technical solutions：A kind of preparation method of composite plant Shu Min agent, including such as Lower step：

(1) wild chrysanthemum flavones and preservative are dispersed with stirring in polyalcohol, at a certain temperature homogeneous, obtain mixture I；

(2) Forsythia volatile oil, grease and emulsifier are mixed and are uniformly dispersed, obtain mixtures II；

(3) Honegsukle flower P.E and water are mixed and are uniformly dispersed, obtain mixtures III；

(4) mixture I and mixtures III are sufficiently mixed, mixtures II is added under certain mixing speed, homogeneous obtains To composite plant Shu Min agent.

In step (1)：

The wild chrysanthemum flavones can select commercially available, can also voluntarily prepare, and the stability based on functional component considers, It extracts to obtain preferably by following steps：Using commercially available dry product Chrysanthemum Indicum L. Flower of Huangshan as raw material, absolute ethyl alcohol is as solvent, feed liquid matter Measure ratio 1:(15~30) (g/mL), 50~70 DEG C of water-baths, the stirring of 100~200rpm rotating speeds extract 2~3h, by filtrate after filtering Freeze-drying, obtains wild chrysanthemum flavones.

Content >=85% of general flavone in the wild chrysanthemum flavones；

The composition of active ingredient is as shown in table 1 in the wild chrysanthemum flavones：

Table 1

Sequence number	Component	Content (%)
			1	Luteolin	≥30
2	Quercetin	≥20
			3	Luteolin glucoside	≥10
4	Quercetin glucoside	≥8
			5	Apiolin	≥15

The preservative is preferably one or both of methyl hydroxybenzoate and Nipasol.

The dosage of the preservative meets relevant safety standard, and dosage is by being equivalent to the composite plant Shu Min agent The 0~0.10% of quality calculates；Preferably calculated by 0.05~0.10%.

The dosage of the wild chrysanthemum flavones is calculated by be equivalent to the composite plant Shu Min agent quality 0.5~1%.

The function of the polyalcohol is solvent and assistant for emulsifying agent, is preferably propylene glycol, glycerine, n-butanol, erythrose One or several kinds in alcohol and xylitol.

The dosage of the polyalcohol is calculated by be equivalent to the composite plant Shu Min agent quality 10~12%.

The preferred super-high-pressure homogenization of the homogeneous, condition are as follows：Pressure is 500~800bar；Temperature≤25 DEG C are preferably 20℃；Time is 5~15min.

In step (2)：

The Forsythia volatile oil can select commercially available, can also voluntarily prepare, and the stability based on functional component considers, It is preferred that it is made by the steps to obtain：Using dry product Fructus Forsythiae as raw material, butane carries out subcritical fluid extraction as extractant, Fructus Forsythiae heap 0.5~0.8Kg/L of density, extracting pressure be 0.3~0.4MPa, 40~50 DEG C of extraction temperature, extraction time 30~ 60min after extraction mixed liquor filtering, is evaporated under reduced pressure recycling extractant, obtains Forsythia volatile oil.

The composition of active ingredient is as shown in table 2 in the Forsythia volatile oil：

Table 2

Sequence number	Component	Content (%)
			1	Nopinene	≥20
2	Geraniol	≥10
			3	1- terpinols -4	≥10

The dosage of the Forsythia volatile oil is calculated by be equivalent to the composite plant Shu Min agent quality 2~5%.

The grease can be Synthetic Oil, as isopropyl myristate, isopropyl palmitate, isopropyl stearate, The different monooctyl ester of myristic acid, isobutyl palmitate, three caprylic/capric glyceride, myristic acid nutmeg alcohol ester, isononyl isononanoate Deng；Can also be natural plant grease, such as coconut oil, palm oil, palm-kernel oil, wheat-germ oil, olive oil, castor oil, big Soya-bean oil, grape seed oil, Sweet Almond Oil, camellia oil etc..The preferred natural plant grease of the present invention, more preferably camellia oil.

The camellia oil is commercially available cosmetics-stage camellia oil, is preferably plant of the camellia seed as obtained by cold press extraction Oil.

The quality index of the camellia oil is as shown in table 3：

Table 3

Sequence number	Component	Index
			1	Tocopherol	≥200ppm
2	Tea polyphenols	≥50ppm
			3	Peroxide value	＜ 2.5meq/Kg
4	Acid value	＜ 0.8mgKOH/g

The dosage of the grease is calculated by be equivalent to the composite plant Shu Min agent quality 8~10%.

The emulsifier be preferably Tween-80, Tween-85, Emulsifier EL-60, Crodaret, One or more of ceteth -20 and different ceteth -20；Preferably Tween-80 and different ceteth -20 is answered Close object, mass ratio 1:1.

The dosage of the emulsifier is calculated by be equivalent to the composite plant Shu Min agent quality 5~8%.

The mixing, which is uniformly dispersed, to be carried out by stirring, and mixing speed is preferably 100~200rpm.

In step (3)：

The Honegsukle flower P.E can select commercially available, can also voluntarily prepare, the stability based on functional component is examined Consider, be preferably made by the steps to obtain：Using dry product honeysuckle as raw material, water is as solvent, feed liquid mass ratio 1：(20~ 40), 50~70 DEG C of water-baths, 100~200rpm rotating speeds stirring, extract 2~3h, are freeze-dried filtrate after filtering, obtain gold and silver Flower extract.

The composition of active ingredient is as shown in table 4 in the Honegsukle flower P.E：

Table 4

Sequence number	Component	Content (%)
			1	Chlorogenic acid	≥15
2	Luteolin	≥20
			3	Total reducing sugar	20~40

The dosage of the Honegsukle flower P.E is calculated by be equivalent to the composite plant Shu Min agent quality 1~3%.

The water is preferably deionized water.

The dosage of the water is except wild chrysanthemum flavones, polyalcohol, preservative, Fructus Forsythiae volatilization in composite plant Shu Min agent Oil, grease, the amount outside Honegsukle flower P.E are surplus.

In step (4)：

Described being sufficiently mixed is carried out by stirring, and mixing speed is preferably 100~200rpm.

Mixing speed in certain mixing speed is preferably 300~400rpm.

A kind of composite plant Shu Min agent, is obtained by above-mentioned preparation method.

The composite plant Shu Min agent is suitble to the application in cosmetics, has effects that Shu Min.

The present invention is had the following advantages compared with the prior art and effect：

(1) different deliquescent plant functional components are combined with each other by the present invention by microemulsion technology, add lipophilic The dissolubility of property and hydrophily Shu Min ingredients, can play Shu Min effects at many levels from water phase, oil phase；

(2) present invention preferably camellia oil is as micro emulsion oil phase raw material, compared with other common natural oils, as peanut oil, The micro emulsion grain size smaller of the preparations such as soybean oil, olive oil, since the grain size of micro emulsion is small, is evenly distributed, and in emulsifier and helps emulsification Under the Penetration enhancing effect of agent, various Shu Min ingredients is made to be easier to be absorbed by the skin, Shu Min effects are good；

(3) the preparation method simple process and low cost of micro emulsion of the present invention, is easy to industrialized production.

Specific embodiment

With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.

Embodiment 1

First, the preparation of composite plant Shu Min agent 1, specific technical solution are as follows：

(1) dry product wild chrysanthemum is taken, using absolute ethyl alcohol as solvent, solid-liquid ratio 1:20 (g/ml), 60 DEG C of water-baths, 200rpm turn Filtrate, after filtering is freeze-dried, obtains wild chrysanthemum flavones, detected through HPLC, the results are shown in Table 5, general flavone by speed stirring 2h Content is 90.8%.

Table 5

Sequence number	Component	Content (%)
			1	Luteolin	30.5
2	Quercetin	21.8
			3	Luteolin glucoside	12.4
4	Quercetin glucoside	10.5
			5	Apiolin	15.6

(2) dry product Fructus Forsythiae is taken, subcritical abstraction, Fructus Forsythiae heap density 0.7kg/L, extraction are carried out using butane as extractant After extraction mixed liquor filtering, recycling extractant is evaporated under reduced pressure in pressure 0.4MPa, 45 DEG C, extraction time 50min of extraction temperature, Obtain Forsythia volatile oil.It is detected through GC, the results are shown in Table 6.

Table 6

Sequence number	Component	Content (%)
			1	Nopinene	22.5
2	Geraniol	12.1
			3	1- terpinols -4	11.8

(3) dry product honeysuckle is taken, using water as solvent, feed liquid mass ratio 1:20 (g/ml), 70 DEG C of water-baths, 200rpm rotating speeds 2h is stirred, filtrate is freeze-dried after filtering, obtains Honegsukle flower P.E.Chlorogenic acid and Luteolin content are detected with HPLC, Polyoses content is measured with anthrone method, the results are shown in Table 7.

Table 7

Sequence number	Component	Content (%)
			1	Chlorogenic acid	15.5
2	Luteolin	23.4
			3	Total reducing sugar	25.7

(4) 10 mass parts antierythrites, 0.5 mass parts wild chrysanthemum flavones, 0.025 mass parts methyl hydroxybenzoate, 0.025 matter are taken Part Nipasol is measured, in 500bar, temperature is super-high-pressure homogenization 5min at 20 DEG C, obtains mixture I；8 mass parts camellia oils are taken, 2 mass parts Forsythia volatile oils, 2.5 mass parts Tween-80s, different ceteth -20 of 2.5 mass parts are mixed under 100rpm rotating speeds Conjunction is uniformly dispersed, and obtains mixtures II；Take 73 mass parts deionized waters, 1 mass parts Honegsukle flower P.E, under 100rpm rotating speeds Mixing is uniformly dispersed, and obtains mixtures III；Mixture I and III is uniformly mixed under the stirring of 100rpm rotating speeds, by stirring speed Degree is promoted to 300rpm, is added in mixtures II and is uniformly mixed, the super-high-pressure homogenization 5min at pressure 500bar, 20 DEG C of temperature is obtained Composite plant Shu Min agent 1.

2nd, the preparation of micro emulsion 1.1 is compareed：

Take 10.5 mass parts antierythrites, 0.025 mass parts methyl hydroxybenzoate, 0.025 mass parts Nipasol, 500bar, temperature are super-high-pressure homogenization 5min at 20 DEG C, obtain mixture I；Take 10 mass parts camellia oils, 2.5 mass parts tweens- 80th, different ceteth -20 of 2.5 mass parts are uniformly mixed under the stirring of 100rpm rotating speeds, obtain mixtures II；By mixture I, 74 mass parts deionized water is uniformly mixed under the stirring of 100rpm rotating speeds, and mixing speed is promoted to 300rpm, adds in mixture II, the super-high-pressure homogenization 5min at pressure 500bar, 20 DEG C of temperature, must compare micro emulsion 1.1.

3rd, the preparation of micro emulsion 1.2 and 1.3 is compareed

Compare the preparation of micro emulsion 1.2：Preparation process and step 1 differ only in：With the commercially available olive of identical mass parts Oil replaces camellia oil.

Compare the preparation of micro emulsion 1.3：Preparation process and step 1 differ only in：With the soybean oil generation of identical mass parts For camellia oil.

Embodiment 2

First, the preparation of composite plant Shu Min agent 2, specific technical solution are as follows：

(1) dry product wild chrysanthemum is taken, using absolute ethyl alcohol as solvent, solid-liquid ratio 1:30 (g/ml), 50 DEG C of water-baths, 100rpm turn Filtrate, after filtering is freeze-dried, obtains wild chrysanthemum flavones, detected through HPLC, the results are shown in Table 8, general flavone by speed stirring 3h Content is 89.8%.

Table 8

Sequence number	Component	Content (%)
			1	Luteolin	30.2
2	Quercetin	20.5
			3	Luteolin glucoside	12.5
4	Quercetin glucoside	10.8
			5	Apiolin	15.8

(2) dry product Fructus Forsythiae is taken, subcritical abstraction, Fructus Forsythiae heap density 0.5kg/L, extraction are carried out using butane as extractant After extraction mixed liquor filtering, recycling extractant is evaporated under reduced pressure in pressure 0.3MPa, 40 DEG C, extraction time 30min of extraction temperature, Obtain Forsythia volatile oil.After testing, the results are shown in Table 9.

Table 9

Sequence number	Component	Content (%)
			1	Nopinene	21.4
2	Geraniol	12.5
			3	1- terpinols -4	10.9

(3) dry product honeysuckle is taken, using water as solvent, feed liquid mass ratio 1:30 (g/ml), 60 DEG C of water-baths, 150rpm rotating speeds 2.5h is stirred, filtrate is freeze-dried after filtering, obtains Honegsukle flower P.E.After testing, the results are shown in Table 10.

Table 10

Sequence number	Component	Content (%)
			1	Chlorogenic acid	16.2
2	Luteolin	22.7
			3	Total reducing sugar	27.9

(4) 12 mass parts glycerine, 1 mass parts wild chrysanthemum flavones, 0.05 mass parts methyl hydroxybenzoate, 0.05 mass parts hydroxyl are taken Phenylpropyl alcohol ester, in 800bar, temperature is super-high-pressure homogenization 15min at 20 DEG C, obtains mixture I；Take 10 mass parts camellia oils, 5 matter Part Forsythia volatile oil is measured, 4 mass parts Tween-80s, different ceteth -20 of 4 mass parts mix scattered equal under 200rpm rotating speeds It is even, obtain mixtures II；Take 60.9 mass parts deionized waters, 3 mass parts Honegsukle flower P.Es, the mixing point under 200rpm rotating speeds It dissipates uniformly, obtains mixtures III；Mixture I and III under the stirring of 200rpm rotating speeds is uniformly mixed, mixing speed is promoted To 400rpm, add in mixtures II and be uniformly mixed, the super-high-pressure homogenization 15min at pressure 800bar, 20 DEG C of temperature obtains compound plant Object Shu Min agent 2.

2nd, the preparation of micro emulsion 2.1 is compareed：

Take 13 mass parts glycerine, 0.05 mass parts methyl hydroxybenzoate, 0.05 mass parts Nipasol, in 800bar, temperature For super-high-pressure homogenization 15min at 20 DEG C, mixture I is obtained；Take 15 mass parts camellia oils, 4 mass parts Tween-80s, 4 mass parts different Ceteth -20 are uniformly mixed under the stirring of 200rpm rotating speeds, obtain mixtures II；Mixture I, 60.9 mass parts are gone Ionized water is uniformly mixed under the stirring of 200rpm rotating speeds, and mixing speed is promoted to 400rpm, mixtures II is added in, in pressure 800bar, super-high-pressure homogenization 15min at 20 DEG C of temperature, must compare micro emulsion 2.1.

3rd, the preparation of micro emulsion 2.2 and 2.3 is compareed

Compare the preparation of micro emulsion 2.2：Preparation process and step 1 differ only in：With the commercially available olive of identical mass parts Oil replaces camellia oil.

Compare the preparation of micro emulsion 2.3：Preparation process and step 1 differ only in：With the soybean oil generation of identical mass parts For camellia oil.

Embodiment 3

First, the preparation of composite plant Shu Min agent 3, specific technical solution are as follows：

(1) dry product wild chrysanthemum is taken, using absolute ethyl alcohol as solvent, solid-liquid ratio 1:15 (g/ml), 70 DEG C of water-baths, 150rpm turn Filtrate, after filtering is freeze-dried, obtains wild chrysanthemum flavones by speed stirring 2.5h.After testing, as a result as shown in table 11, general flavone contains It measures as 91.0%.

Table 11

Sequence number	Component	Content (%)
			1	Luteolin	30.7
2	Quercetin	20.5
			3	Luteolin glucoside	13.1
4	Quercetin glucoside	10.6
			5	Apiolin	16.1

(2) dry product Fructus Forsythiae is taken, subcritical abstraction, Fructus Forsythiae heap density 0.8kg/L, extraction are carried out using butane as extractant After extraction mixed liquor filtering, recycling extractant is evaporated under reduced pressure in pressure 0.35MPa, 50 DEG C, extraction time 60min of extraction temperature, Obtain Forsythia volatile oil.After testing, as a result as shown in table 12.

Table 12

Sequence number	Component	Content (%)
			1	Nopinene	21.6
2	Geraniol	12.5
			3	1- terpinols -4	10.3

(3) dry product honeysuckle is taken, using water as solvent, feed liquid mass ratio 1:40 (g/ml), 50 DEG C of water-baths, 100rpm rotating speeds 3h is stirred, filtrate is freeze-dried after filtering, obtains Honegsukle flower P.E.After testing, as a result as shown in table 13.

Table 13

Sequence number	Component	Content (%)
			1	Chlorogenic acid	15.8
2	Luteolin	22.7
			3	Total reducing sugar	29.3

(4) 11 mass parts xylitols, 0.8 mass parts wild chrysanthemum flavones, 0.04 mass parts methyl hydroxybenzoate, 0.04 mass parts are taken Nipasol, in 700bar, temperature is super-high-pressure homogenization 10min at 20 DEG C, obtains mixture I；Take 9 mass parts camellia oils, 3 matter Part Forsythia volatile oil is measured, 3 mass parts Tween-80s, different ceteth -20 of 3 mass parts mix scattered equal under 150rpm rotating speeds It is even, obtain mixtures II；68.12 mass parts deionized waters are taken, 2 mass parts Honegsukle flower P.Es mix under 150rpm rotating speeds It is uniformly dispersed, obtains mixtures III；Mixture I and III under the stirring of 150rpm rotating speeds is uniformly mixed, mixing speed is carried 350rpm is raised to, mixtures II is added in and is uniformly mixed, the super-high-pressure homogenization 10min at pressure 700bar, 20 DEG C of temperature is obtained compound Plant Shu Min agent 3.

2nd, the preparation of micro emulsion 3.1 is compareed：

Take 11.8 mass parts xylitols, 0.04 mass parts methyl hydroxybenzoate, 0.04 mass parts Nipasol, in 700bar, temperature It spends for super-high-pressure homogenization 10min at 20 DEG C, obtains mixture I；Take 12 mass parts camellia oils, 3 mass parts Tween-80s, 3 mass parts Different ceteth -20 are uniformly mixed under the stirring of 150rpm rotating speeds, obtain mixtures II；By mixture I, 74.12 mass parts Deionized water is uniformly mixed under the stirring of 150rpm rotating speeds, and mixing speed is promoted to 350rpm, mixtures II is added in, in pressure 700bar, super-high-pressure homogenization 10min at 20 DEG C of temperature, must compare micro emulsion 3.1.

3rd, the preparation of micro emulsion 3.2 and 3.3 is compareed

Compare the preparation of micro emulsion 3.2：Preparation process and step 1 differ only in：With the commercially available olive of identical mass parts Oil replaces camellia oil.

Compare the preparation of micro emulsion 3.3：Preparation process and step 1 differ only in：With the soybean oil generation of identical mass parts For camellia oil.

Embodiment test evaluation

1. safety evaluatio

Skin irritation test

The healthy Adult New Zealand White Rabbit 18 without skin injury is chosen, divides intact skin (9) and damaged skin group (9) are tested, lacing number according to the method that rabbit itself left and right sides skin compares.For 24 hours among rabbit back before experiment The skin depilatory of backbone both sides, per side hair removal section with 16cm²Left and right is advisable.Observation rabbit whether there is Novel presentation afterwards for 24 hours for depilation.It is broken Damage skin group is scratched the depilation skin after disinfection with pin, is advisable with oozing of blood.

Composite plant Shu Min agent 1 prepared by 1ml embodiments 1 is taken uniformly to be applied to intact skin group 1~3 and breakage respectively The left side hair removal section of 1~No. 3 rabbit of skin group, take respectively 1ml control micro emulsion 1.1 be uniformly applied to skin completely group 1~No. 3 and The right side hair removal section of 1~No. 3 rabbit of skin injury group；Composite plant Shu Min agent 2 prepared by 1ml embodiments 2 is taken uniformly to apply respectively Skin completely group 4~6 and the left side hair removal section of 4~No. 6 rabbits of skin injury group are put on, takes 1ml control micro emulsions 2.1 equal respectively It is even to be applied to skin completely group 4~6 and the right side hair removal section of 4~No. 6 rabbits of skin injury group；1ml embodiments 3 is taken to make respectively Standby composite plant Shu Min agent 3 is uniformly applied to skin, and completely the left side of group 7~9 and 7~No. 9 rabbits of skin injury group is lost hair or feathers Area takes control 3.1 1ml of micro emulsion to be uniformly applied to the skin completely right side of group 7~9 and 7~No. 9 rabbits of skin injury group respectively Side hair removal section.

Skin after smearing is covered with one layer of oilpaper, and covers two layers of gauze on it, is fixed with medical proof fabric, cage is divided to raise Support every group of rabbit.After administration for 24 hours, rabbit hair removal section skin residual sample is washed off with warm water, every hair removal section skin of observation for 24 hours Whether skin there is erythema or oedema, is observed continuously 7 days.

The results show that only damaged organize on the left of No. 5 hair removal sections that sample is interior for 24 hours slight erythema and oedema, 48h occurs smearing Erythema and oedema are gradually taken off afterwards.The activity of remaining rabbit four limbs and left and right hair removal section skin are normal, and intact skin group is androgynous left Right both sides skin compares, and difference is not notable；Damaged skin group consubstantiality left and right sides skin compares, and difference is not notable；Intact skin group Compared with depilation skin on the left of damaged skin group, difference is not notable.It can be considered that the composite plant Shu Min of Examples 1 to 3 Agent is to no skin irritation.

2. estimation of stability

Composite plant Shu Min agent prepared by Example 1~3 is placed in centrifuge tube, with 8000rpm in supercentrifuge Speed centrifugation 20min, observed after taking-up, do not occur precipitating or lamination, illustrate composite plant Shu Min agent high speed from It has good stability in heart experiment.

Composite plant Shu Min agent prepared by Example 1~3 is respectively placed in good seal in 5ml vials, in temperature 40 ± 1 DEG C, it is placed 1 month under conditions of humidity 75% ± 5%, once, all micro emulsion appearances nothing is substantially change, explanation for observation in every 3 days Shu Min stability of microemulsion is good.

3. Efficiency assessment

(1) particle size determination

Control micro emulsion 1.1,1.2,1.3,2.1,2.2,2.3,3.1,3.2,3.3 and composite plant Shu Min agent 1,2,3 are taken, point 20 times are not diluted with water, are measured with Nanophox nano-particle size analysis instrument, it is as shown in table 14 to measure each micro emulsion grain size：

Table 14

Embodiment 1	Composite plant Shu Min agent 1	Compare micro emulsion 1.1	Compare micro emulsion 1.2	Compare micro emulsion 1.3
					Grain size nm	31.67	38.24	57.82	80.71
Embodiment 2	Composite plant Shu Min agent 2	Compare micro emulsion 2.1	Compare micro emulsion 2.2	Compare micro emulsion 2.3
					Grain size nm	32.04	37.13	53.74	80.39
Embodiment 3	Composite plant Shu Min agent 3	Compare micro emulsion 3.1	Compare micro emulsion 3.2	Compare micro emulsion 3.3
					Grain size nm	31.51	36.32	54.55	78.04

As it can be seen that under the preferred each group distribution ratio of the micro emulsion and preferred preparation method, the institute using camellia oil as oil phase The micro emulsion grain size obtained is all smaller than the micro emulsion obtained by olive oil and soybean oil, is more advantageous to being absorbed by the skin.

(2) vitro Transdermal

The disconnected neck of male Sprague Dawley rats (150~300g of weight) is taken to put to death, skin of abdomen is removed, uses electric shaving Must knife cut off mouse hair, subcutaneous tissue adhesion object is cut with mechanical shear, then subcutaneus adipose tissue is wiped with isopropanol, with water by isopropyl Alcohol is rinsed well, is immersed in physiological saline, freezen protective, for use.By mouse leather jacket on Franz diffusion cells, court on the outside of mouse skin To supply pool, the physiological saline containing 10% (v/v) Tween-80 is filled it up in reception tank, has magnet rotor, rotating speed in reception tank 200rpm keeps 37 ± 1 DEG C of temperature, and 4ml samples are added in supply pool, takes solution in reception tank after 6h, according to document "《Change The screening of cosmetic antiallergic anti-irritant active material extracts and makees mechanism study》[D] Wang Haitao Beijing Technology and Business Universitys, 2010: Hyaluronidase in vitro method in 75-81 " measures solution in reception tank and, to the inhibiting rate of hyaluronidase, sentences on this basis Shu Min effects after disconnected sample Transdermal absorption.

Test sample has composite plant Shu Min agent 1, compares micro emulsion 1.2, compares micro emulsion 1.3, and sample 1 (contains 2% mass point The camellia oil of Forsythia volatile oil prepared by number embodiment 1, i.e., mix 0.2 mass parts Forsythia volatile oil and 9.8 mass parts camellia oils It is even to be made), (the antierythrite solution containing wild chrysanthemum flavones prepared by 0.5% mass fraction embodiment 1, i.e., by 0.05 of sample 2 Mass parts wild chrysanthemum flavones and 9.95 mass parts antierythrite mixings are made), sample 3 (is made containing 1% mass fraction embodiment 1 The deionized water of standby Honegsukle flower P.E, i.e., by 0.1 mass parts Honegsukle flower P.E and 9.9 mass parts deionized water mixing systems ).In addition set one group first to add 4ml samples 1 (camellia oil for containing 2% Forsythia volatile oil), outwell solution in supply pool after 6h, add Enter 4ml samples 2 (the antierythrite solution for containing 0.5% wild chrysanthemum flavones), outwell solution in supply pool after 6h, add in 4ml samples 3 The deionized water solution of 1% Honegsukle flower P.E (contain) takes liquid in reception tank to do the test of hyaluronidase in vitro method after 6h.Often Group sample sets parallel group 3, calculates inhibiting rate average value.

Test result is as shown in Table 15：

Table 15

After Transdermal absorption, the inhibition hyaluronidase rate that composite plant Shu Min agent 1 relatively compares micro emulsion 1.2 and 1.3 is high, It is more easily absorbed by the skin it can be seen that micro emulsion grain size is smaller；Shu Min micro emulsions group is compared with the inhibition hyalomitome of single plant Shu Min ingredients Sour enzyme rate is high, this, which embodies Shu Min micro emulsions, to play the role of Shu Min at many levels from water phase oil phase etc., there is preferable Shu Min effects；It relaxes The quick group of inhibition hyaluronidase rate compared with 3 kinds of plant Shu Min ingredients is high, and embodying microemulsion system is easier plant Shu Min ingredients It is absorbed by the skin.

Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims

1. a kind of preparation method of composite plant Shu Min agent, it is characterised in that include the following steps：

(4) mixture I and mixtures III are sufficiently mixed, mixtures II is added under certain mixing speed, homogeneous is answered Close plant Shu Min agent.

2. the preparation method of composite plant Shu Min agent according to claim 1, it is characterised in that：

The composition of active ingredient is by mass percentage, as follows in wild chrysanthemum flavones described in step (1)：Luteolin >= 30%th, Quercetin >=20%, Luteolin glucoside >=10%, Quercetin glucoside >=8%, apiolin >=15%；

The composition of active ingredient is by mass percentage, as follows in Forsythia volatile oil described in step (2)：Nopinene >= 20%th, geraniol >=10%, 1- terpinols -4 >=10%；

The composition of active ingredient is by mass percentage, as follows in Honegsukle flower P.E described in step (3)：Chlorogenic acid >= 15%th, Luteolin >=20%, total reducing sugar 20~40%.

3. the preparation method of composite plant Shu Min agent according to claim 2, it is characterised in that：

The wild chrysanthemum flavones extracts to obtain as follows：Using commercially available dry product Chrysanthemum Indicum L. Flower of Huangshan as raw material, absolute ethyl alcohol As solvent, feed liquid mass ratio 1:(15~30), 50~70 DEG C of water-baths, the stirring of 100~200rpm rotating speeds extract 2~3h, filtering Filtrate is freeze-dried afterwards, obtains wild chrysanthemum flavones；

The Forsythia volatile oil is made by the steps to obtain：Using dry product Fructus Forsythiae as raw material, butane as extractant into Row subcritical fluid extraction, Fructus Forsythiae heap 0.5~0.8Kg/L of density, extracting pressure be 0.3~0.4MPa, extraction temperature 40~50 DEG C, 30~60min of extraction time after extraction mixed liquor filtering, is evaporated under reduced pressure recycling extractant, obtains Forsythia volatile oil；

The Honegsukle flower P.E is made by the steps to obtain：Using dry product honeysuckle as raw material, water is as solvent, feed liquid Mass ratio 1：(20~40), 50~70 DEG C of water-baths, the stirring of 100~200rpm rotating speeds extract 2~3h, freeze filtrate after filtering It is dry, obtain Honegsukle flower P.E.

4. the preparation method of composite plant Shu Min agent according to claim 1, it is characterised in that：

The dosage of the wild chrysanthemum flavones is calculated by be equivalent to the composite plant Shu Min agent quality 0.5~1%；

The dosage of the polyalcohol is calculated by be equivalent to the composite plant Shu Min agent quality 10~12%；

The dosage of the preservative is calculated by be equivalent to the composite plant Shu Min agent quality 0~0.10%；

The dosage of the Forsythia volatile oil is calculated by be equivalent to the composite plant Shu Min agent quality 2~5%；

The dosage of the grease is calculated by be equivalent to the composite plant Shu Min agent quality 8~10%；

The dosage of the emulsifier is calculated by be equivalent to the composite plant Shu Min agent quality 5~8%；

The dosage of the Honegsukle flower P.E is calculated by be equivalent to the composite plant Shu Min agent quality 1~3%；

The water is surplus.

5. the preparation method of composite plant Shu Min agent according to claim 4, it is characterised in that：The use of the preservative Amount is calculated by be equivalent to the composite plant Shu Min agent quality 0.05~0.10%.

6. the preparation method of composite plant Shu Min agent according to claim 1, it is characterised in that：

The preservative is one or both of methyl hydroxybenzoate and Nipasol；

The polyalcohol is the one or several kinds in propylene glycol, glycerine, n-butanol, antierythrite and xylitol；

The grease is isopropyl myristate, isopropyl palmitate, isopropyl stearate, the different monooctyl ester of myristic acid, palm The different monooctyl ester of acid, three caprylic/capric glyceride, myristic acid nutmeg alcohol ester, isononyl isononanoate, coconut oil, palm oil, palm One or more of benevolence oil, wheat-germ oil, olive oil, castor oil, soybean oil, grape seed oil, Sweet Almond Oil and camellia oil；

The emulsifier is Tween-80, Tween-85, Emulsifier EL-60, Crodaret, cetanol gather One or more of ether -20 and different ceteth -20.

7. the preparation method of composite plant Shu Min agent according to claim 6, it is characterised in that：

The grease is camellia oil；

The emulsifier is Tween-80 and different ceteth -20 in mass ratio 1:1 obtained compound.

8. the preparation method of composite plant Shu Min agent according to claim 1, it is characterised in that：

The condition of homogeneous described in step (1) and step (4) is as follows：Pressure is 500~800bar, temperature≤25 DEG C, time For 5~15min；

Mixing described in step (2) and step (3), which is uniformly dispersed, to be carried out by stirring, and mixing speed is 100~200rpm；

Described being sufficiently mixed is carried out by stirring, and mixing speed is 100~200rpm；

Mixing speed in certain mixing speed is 300~400rpm.

9. a kind of composite plant Shu Min agent, it is characterised in that：It is obtained by claim 1~8 any one of them preparation method.

10. application of the composite plant Shu Min agent in cosmetics described in claim 9.