Summary of the invention
The first technical problem to be solved by the present invention is: providing, a kind of synergistic function is good to be mentioned containing blueberry
Take the antiseptic composition of object.
Second technical problem to be solved by this invention is: providing the above-mentioned preservative combination containing myrtillin chloride
The preparation method of object.
Third technical problem to be solved by this invention is: providing the above-mentioned preservative combination containing myrtillin chloride
The application of object.
In order to solve above-mentioned first technical problem, the technical solution adopted by the present invention are as follows: one kind is extracted containing blueberry
The antiseptic composition of object, the antiseptic composition are made of myrtillin chloride, synergetic effect additive and solvent, the collaboration
Synergist includes at least one of polyalcohol or aromatic alcohol, and the solvent includes at least one of alcohol or water;
The weight percentage of the myrtillin chloride be 2~28%, synergetic effect additive weight percentage be 3~
55%, solvent is surplus.
Preferably, the weight percentage of the myrtillin chloride is 10~20%, it is highly preferred that weight percentage
It is 12~15%.
Preferably, the weight percentage of the synergetic effect additive is 45~50%.
Further, at least contain four carbon atom in the polyalcohol.
Further, the polyalcohol is alkylol.
Preferably, the synergetic effect additive include 1,2- butanediol, 1,2- hexylene glycol, 1,2- ethohexadiol, 1,2- decanediol,
At least one of benzyl carbinol, benzylalcohol or Sensiva SC50.
Further, the solvent includes at least one of 1,2-PD, glycerine, polyethylene glycol or water.
The beneficial effects of the present invention are: the composition stability of the present invention program is good, mentions in composition containing blueberry
Taking object is that the other natural plant preservative of edible grade is small to injury of human, and synergetic effect additive is alcohols material, and solvent is also alcohol
Substance or water, simultaneously as alcohols material itself also has fungistatic effect, synergetic effect additive and solvent can not only improve crow
The dissolution of Polyphenols, Flavonoid substances in meal tree extract, can also enhance its fungistatic effect to bacterium, promote it to fungi
Bacteriostasis;In addition, the Polyphenols or Flavonoid substances in myrtillin chloride also have stronger antioxidation, therefore,
The composition of the present invention program also has good antioxidation in addition to bacteriostasis.
In order to solve above-mentioned second technical problem, the technical solution adopted by the present invention are as follows: one kind is extracted containing blueberry
The preparation method of the antiseptic composition of object, comprising the following steps: after mixing myrtillin chloride and solvent, add collaboration
Synergist, is warming up to 35~60 DEG C, stirring to it is complete it is molten after, be cooled to room temperature to obtain the final product.
Preferably, the preparation process of the myrtillin chloride is as follows:
Coarse extraction is carried out to blueberry leaf using ultrasound-microwave extraction method, then uses response surface, with flavonoids, Polyphenols
Substance recovery rate is evaluation index, is higher than 5% with Vaccinium bracteatum Thunb. Leaves flavones yield, it is mesh that blueberry leaf polyphenol yield, which is higher than 3%,
Mark, optimizes technique.
Preferably, the process conditions of the ultrasound-microwave extraction method are as follows: microwave power 140W, temperature are 70 DEG C, and liquid is solid
Than for 50 (mL/g), extraction time 12min.
Further, the preparation process of the myrtillin chloride further include: refined using nanofiltration membrane.
Further, the operating pressure in the subtractive process is 0.5MPa.
The beneficial effects of the present invention are: the preparation process of the antiseptic composition of the present invention program is easy.Using ultrasound-
Microwave extraction method prepares myrtillin chloride, and the residual quantity of solvent can be greatly decreased.
In order to solve above-mentioned third technical problem, the technical solution adopted by the present invention are as follows: one kind is above-mentioned to contain blueberry
Application of the antiseptic composition of extract in the preparation of cosmetics.
The beneficial effects of the present invention are: the composition of the present invention program is added in cosmetics, biography can not only be substituted
System chemical preservative is added in cosmetics, plays the role of antiseptic and inhibiting bacteria function, while also having the effect of beautifying face and moistering lotion.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, below in conjunction with embodiment and cooperate attached
Figure is explained.
The embodiment of the present invention one are as follows: a kind of antiseptic composition, by myrtillin chloride, synergetic effect additive and solvent group
At, wherein the synergetic effect additive is by 1,2- ethohexadiol and 1, and 2- butanediol composition, the solvent is by 1,2-PD and water group
At.Wherein, the quality accounting of the myrtillin chloride is 9%, and the quality accounting of synergetic effect additive is 35%, and solvent is remaining
Amount.1,2- ethohexadiol and 1, the mass ratio of 2- butanediol are 5:2, and the quality accounting of 1,2-PD and water is 15:13.
The embodiment of the present invention two are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of benzyl carbinol and Sensiva SC50, and the solvent is made of 1,2-PD and polyethylene glycol.Wherein, the black meal
The quality accounting for setting extract is 12%, and the quality accounting of synergetic effect additive is 42%, and solvent is surplus.Benzyl carbinol and ethyl hexyl
The mass ratio of base glycerol is 4:10, and the quality accounting of 1,2-PD and polyethylene glycol is 25:26.
The embodiment of the present invention three are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of benzyl carbinol and 1,2- butanediol composition, the solvent water and polyethylene glycol.Wherein, the myrtillin chloride
Quality accounting is 14%, and the quality accounting of synergetic effect additive is 39%, and solvent is surplus.The quality of benzyl carbinol and 1,2- butanediol
Than for 1:2, the quality accounting of water and polyethylene glycol is 20:27.
The embodiment of the present invention four are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is 1,2-PD by Sensiva SC50 and 1,2- ethohexadiol composition, the solvent.Wherein, the myrtillin chloride
Quality accounting is 10%, and the quality accounting of synergetic effect additive is 60%, and solvent is surplus.Sensiva SC50 and 1,2- ethohexadiol
Mass ratio be 33:27.
The embodiment of the present invention five are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of benzylalcohol, 1,2- decanediol and 1,2- ethohexadiol composition, the solvent water and 1,2-PD.Wherein, the crow
The quality accounting of meal tree extract is 25%, and the quality accounting of synergetic effect additive is 38%, and solvent is surplus.Benzylalcohol, the 1,2- last of the ten Heavenly stems
The mass ratio of two pure and mild 1,2- ethohexadiols is 9:4:6, and the quality accounting of water and 1,2-PD is 12:25.
The embodiment of the present invention six are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of 1,2- decanediol and 1,2- butanediol composition, the solvent water and 1,2-PD.Wherein, the blueberry mentions
The quality accounting for taking object is 16%, and the quality accounting of synergetic effect additive is 33%, and solvent is surplus.Decane-1,2-diol and 1,2- fourth
The mass ratio of glycol is 20:13, and the quality accounting of water and 1,2-PD is 29:20.
The embodiment of the present invention seven are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of benzylalcohol and 1,2- butanediol composition, the solvent polyethylene glycol and 1,2-PD.Wherein, the blueberry mentions
The quality accounting for taking object is 4%, and the quality accounting of synergetic effect additive is 30%, and solvent is surplus.Benzylalcohol and 1,2- butanediol
Mass ratio is 8:7, and the quality accounting of polyethylene glycol and 1,2-PD is 25:41.
The embodiment of the present invention eight are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of 1,2- butanediol, 1,2- ethohexadiol and 1,2- decanediol composition, the solvent polyethylene glycol and water.Wherein, institute
The quality accounting for stating myrtillin chloride is 24%, and the quality accounting of synergetic effect additive is 23%, and solvent is surplus.1,2- fourth two
Alcohol, 1,2- ethohexadiol and 1, the mass ratio of 2- decanediol are 11:6:6, and the quality accounting of polyethylene glycol and water is 33:20.
The embodiment of the present invention nine are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of 1,2- butanediol, benzyl carbinol and benzylalcohol, and the solvent is made of polyethylene glycol and 1,2-PD.Wherein, described
The quality accounting of myrtillin chloride is 2%, and the quality accounting of synergetic effect additive is 37%, and solvent is surplus.1,2- butanediol,
The mass ratio of benzyl carbinol and benzylalcohol is 12:10:15, and the quality accounting of polyethylene glycol and 1,2-PD is 43:18.
The embodiment of the present invention ten are as follows: a kind of antiseptic composition, the difference with embodiment one are: the synergy
Agent is made of 1,2- butanediol and Sensiva SC50, and the solvent is made of water and 1,2-PD.Wherein, the blueberry
The quality accounting of extract is 28%, and the quality accounting of synergetic effect additive is 30%, and solvent is surplus.1,2- butanediol and ethyl
The mass ratio of hexyl glycerol is 1:1, and the quality accounting of water and 1,2-PD is 2:5.
The embodiment of the present invention 11 are as follows: a kind of antiseptic composition is with the difference of embodiment one: described to cooperate with increasing
It imitates agent to be made of 1,2- butanediol, 1,2- decanediol and Sensiva SC50, the solvent is 1,2-PD.Wherein, described
The quality accounting of myrtillin chloride is 22%, and the quality accounting of synergetic effect additive is 33%, and solvent is surplus.1,2- fourth two
The mass ratio of alcohol, Decane-1,2-diol and Sensiva SC50 is 5:6:12.
Antiseptic composition in above-described embodiment the preparation method is as follows:
S1, microwave power be 140W, temperature be 70 DEG C, liquid-solid ratio be 50 (mL/g) under conditions of pass through ultrasound-microwave
Extraction prepares myrtillin chloride crude product, extraction time 12min;And it is excessively resistance to the myrtillin chloride obtained after extraction
The nanofiltration membrane of organic solvent is refined, and the lighter of extract is made, and stability enhances, the operation pressure in the subtractive process
Power is 0.5MPa.
S2, myrtillin chloride, synergetic effect additive and solvent are weighed in proportion, myrtillin chloride is first added into container
It is uniform with stirring solvent, synergetic effect additive is added, 60 DEG C or so is warming up to, is down to room temperature after stirring to all dissolutions, obtains
Stable natural plant preservative composition.
For the performance for verifying antiseptic composition made from above-described embodiment, following test is carried out:
1), bacteriostasis is tested:
For the antiseptic property for testing foregoing preservatives composition, bacteriostatic experiment is carried out, determines to press down by inhibition zone measuring method
Bacterium ability.With reference to " sterile products inspection technology specification 2.1.8.2 antibacterial ring size examination in " disinfection technology standard (version in 2002) "
Test ", United States Pharmacopeia USP35-<51>Antimicrobial Effectiveness Testing, " cosmetics health specification
(version in 2015) " " Part IV Micro biological Tests method ".
1, test strain: Escherichia coli (Escherichia coli), staphylococcus aureus
(Staphylococcusaureus), Candida albicans (Candida albicans).
2, test specimen: (myrtillin chloride used in antiseptic composition is female for Example 1-4 antiseptic composition
Liquid concentration is 2%), using 50% propylene glycol as blank control.
Three groups of experiments are carried out in parallel, are averaged as shown in table 1 below:
Antibacterial ring size (mm) of 1 antiseptic composition of table to bacterium and fungi
Inhibition zone diameter is greater than 7mm person, has been judged to bacteriostasis.Inhibition zone diameter is less than or equal to 7mm person, is judged to no suppression
Bacterium effect.3 repetition tests have bacteriostasis result person, are judged to qualification.Upper table sample product all have bacteriostasis.It is black in table 1
Meal tree extract concentrations are 0.3%, are above the myrtillin chloride addition concentration arrived used in 4 groups of antiseptic compositions,
It can be seen that single myrtillin chloride is above blank control to the inhibition zone value of each bacterium, but it is lower than mostly and has added synergy
Agent antiseptic composition (in addition to golden yellow staphylococcus compared with 1# preferably other than, remaining is below the inhibition zone of each antiseptic composition
Value), i.e., the fungistatic effect of the myrtillin chloride antiseptic composition added with synergetic effect additive is mentioned than blueberry is used alone
Take the good antimicrobial effect of object.
2), minimum inhibitory concentration is tested
It is minimum antibacterial dense that Example 1-4 antiseptic composition by spread plate measures each formula antiseptic composition
It spends (minimum inhibitory concentration, MIC value), as shown in table 2 below:
2 preservative lowest bacteria fogging-resistant concentration determining (MIC value) of table
From Table 2, it can be seen that each antiseptic composition MIC value is low compared with single myrtillin chloride MIC value, explanation
Antiseptic composition fungistatic effect is better than myrtillin chloride single-item, can reduce the usage amount of myrtillin chloride.
3), estimation of stability
For the stability for studying antiseptic composition, by antiseptic composition prepared by Examples 1 to 4, (number is distinguished
Correspondence markings are 1~4) distinguish and is stored one month under (- 4 DEG C, room temperature, 54 DEG C) and illumination condition at different temperatures, observe it
Stability result is as shown in table 3 below:
3 antiseptic composition stability test result of table
From table 3 it is observed that composition made from the embodiment of the present invention under various conditions variation (low temperature,
Under high temperature, room temperature and illumination condition) it is able to maintain property stabilization.
4), inhibitor effectiveness test (challenge experiment)
With reference to U.S.'s cosmetics, toilet articles and essence association (Cosmetic, Toiletry&Fragrance
Association, CTFA) recommend protective system efficiency evaluation method, carry out 28 days singles connect bacterium challenge experiment.
1, experimental strain: (Escherichia coli (CICC10389), staphylococcus aureus (CICC10384), verdigris are false for bacterium
Monad (CICC21636);Fungi (aspergillus niger (CICC2487), candida albicans bacterium (CICC1965)).It is connect using Mixed Microbes
Kind, bacterium Mixed Microbes suspension 106CFU/mL;Fungi Mixed Microbes suspension 105CFU/mL。
2, test specimen: by formula, (glycerol 10.0%, water 64.5%, 16/octadecanol 1.0%, cetostearyl alcohol are poly-
Ether -20 2.5%, glycerin monostearate 5.0%, white oil 15%, antiseptic composition 2%) preparing cosmetics, wherein anti-corrosion
Agent composition is taken respectively from embodiment 1,2,3,4, and it is A, B, C, D that prepared cosmetics are numbered respectively.
3, sample inoculation: each 2 parts of 30 grams of above-mentioned cosmetics A, B, C, D are weighed respectively, is separately added into 0.2mL mixed cell
Suspension and 0.2mL mixed fungus suspension are uniformly mixed, and sample is saved in (22 ± 2.5 DEG C) of room temperature, and respectively at 0,3,
7, the clump count in 14,21,28 days detection cosmetics, to judge the inhibitor effectiveness of cosmetics.
4, experimental result
In 0,3,7,14,21 and 28 day sample detection of inoculation, the result is shown in tables 4:
Table 4 contains the product of antiseptic composition of the invention
Myrtillin chloride usage amount is 5% in table 4, and challenge test result shows logical using single myrtillin chloride
The time for crossing challenge test is bacterium the 14th day, fungi the 21st day, and usage amount is big.And each antiseptic composition passes through in upper table
Challenging the time is bacterium the 7th day, fungi the 14th day, is indicated above composition fungistatic effect and extracts better than blueberry is used alone
Object.
5), antioxygenic property is tested
Anti-oxidant is the ability that substance has i.e. the oxidation reaction that free radical can be effectively suppressed with low concentration, the mechanism of action
It can be and directly act on free radical, or consume the substance for being easy to generate free radical indirectly, prevent further to react,
Remove the ability of free radical.Flavones and polyphenol hydroxyl degree are high, can be used as the acceptor of free radical and play antioxidation,
Usual ketone, Polyphenols Scavenging ability are stronger.Flavones and polyphenol hydroxyl degree in myrtillin chloride is high, can make
For free radical acceptor and play antioxidation, there is certain reducing power and there is preferable removing energy to DPPH free radical
Power.Therefore, the antioxygenic property of antiseptic composition, specific test process can be verified by the removing power to DPPH free radical
It is as follows:
Antiseptic composition made from embodiment 4 is dissolved with methanol, respectively prepare mass content be 0.05%, 0.1%,
0.15%, 0.2%, 0.25%, 0.3% methanol solution 2mL is separately added into 1, the 1- diphenyl -2- hardship diazanyl of 0.5mmol/L
(2,2-diphenyl-1-picrylhydrazyl, DPPH) methanol solution 2mL after mixing 15s, places 30min, is A with methanol
Reference surveys absorbance in 490nm, is denoted as Ar;2mL methanol is drawn respectively and DPPH mixes 15s, places 30min, is ginseng with methanol
Than surveying absorbance in 517nm, being denoted as A0, and clearance rate is calculated according to the following formula.
In formula: K is DPPH free radical scavenging activity, %.
Antiseptic composition content and DPPH free radical scavenging activity relation curve as shown in Figure 1, from figure 1 it appears that
Antiseptic composition can reach 78% to the clearance rate of DPPH free radical under 0.05% usage amount, and with the increasing of dosage
Add clearance rate that growth trend is presented, but when antiseptic composition dosage is more than after 0.2%, clearance rate no longer increases, it is seen that this
Antiseptic composition has extremely strong antioxidation.
The test result of section Example composition is above only listed, the test result of other embodiments is similar, therefore
It does not repeat.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright specification and accompanying drawing content are applied directly or indirectly in relevant technical field, similarly include
In scope of patent protection of the invention.