CN107224408A - A kind of plant source broad spectrum antimicrobial agent and its preparation method and application - Google Patents
A kind of plant source broad spectrum antimicrobial agent and its preparation method and application Download PDFInfo
- Publication number
- CN107224408A CN107224408A CN201610169716.3A CN201610169716A CN107224408A CN 107224408 A CN107224408 A CN 107224408A CN 201610169716 A CN201610169716 A CN 201610169716A CN 107224408 A CN107224408 A CN 107224408A
- Authority
- CN
- China
- Prior art keywords
- oil
- preparation
- water
- lipase
- plant source
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
- A61K8/602—Glycosides, e.g. rutin
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/66—Enzymes
-
- 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
-
- 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
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Abstract
The invention discloses a kind of plant source broad spectrum antimicrobial agent and its preparation method and application, its raw material includes material A, water, lipase and pH adjusting agent, in terms of 100 parts of mass fraction, material A includes 0.1~5 part of litsea citrate oil, 0.1~5 part of patchouli oil, 0.1~5 part of citronella oil, 0.1~5 part of hydrolysis ginsenoside and 80~99.6 parts of Miglyol 812N；Preparation method is：1) each component in material A is mixed, obtains rich mixture；2) water and lipase are mixed, adjusts pH to 7~10, then mixed with rich mixture, enzymolysis is stirred at 40~50 DEG C；3) ultrasound is carried out to enzymolysis liquid, then water-oil separating takes oil phase；4) ripening is carried out to oil phase, takes supernatant liquid filtering, obtain filtrate, you can.The plant source broad spectrum antimicrobial agent that the present invention is provided has the advantages that small broad-spectrum antiseptic, gentle, good dissolubility, economy, consumption, stabilization and suitable industrialized production.
Description
Technical field
The present invention relates to a kind of plant source broad spectrum antimicrobial agent and its preparation method and application.
Background technology
Preservative refers to the material that microorganism can be prevented to grow.In cosmetics, the effect of preservative is protection product,
It is allowed to from microorganism pollution.Conventional preservative is generally synthetic preservative at present, such as hydantoins (DMDMH), Kathon CG system
Row, Bronopol, iodopropynyl butyl formate (IPBC), parabens, triclosan etc..These preservatives are present
Certain defect：For example, DMDMH easily discharges methanol in use, there is potential safety hazard；Kathon CG series makes because of chlorine-containing component
May some skin quality be produced with certain excitant during；Bronopol is also easy to produce carcinogen nitrosamine；IPBC may
Cause the Excess free enthalpy of user's iodine；Parabens easily produces accumulation in adipose tissue；Triclosan has been found to can be to ring
Border has a negative impact；In addition P-hydroxybenzoic acid antiseptic kind has confirmed in specific test system can show certain mould
Intend the ability of female sex hormone estrogen, safe to the human body and physiological system brings harmful effect.It can be seen that, in the market needs appearance one badly
Plant low toxicity, efficient, free of contamination natural antiseptic agent.
In recent years, in the case where the upsurge of back to nature, enjoyment green and health is impacted, pure natural anti-corrosion is added in cosmetics
Agent has turned into the focus advocated and developed both at home and abroad, and the antibiotic property day of wide, safety non-toxic by force is isolated from natural product extraction
Right preservative turns into the important directions of Future Development.
And the natural antiseptic agent used at present mostly semifinished product, its color is deeper, and smell is denseer, and antimicrobial spectrum is also narrower.Together
When, some Chinese medicines are used in combination rear antibacterial effect and are not so good as after simple, such as Radix Astragali and radix scutellariae mixing match to Escherichia coli, green pus
The bacteriostasis of bacillus and Salmonella is weaker than exclusive use.Therefore, develop a kind of raw material it is natural, can broad-spectrum antiseptic antibacterial
Agent is this area technical barrier urgently to be resolved hurrily.
The content of the invention
The technical problems to be solved by the invention are to overcome natural antiseptic agent antimicrobial spectrum present in prior art narrower
Defect, and there is provided a kind of plant source broad spectrum antimicrobial agent and its preparation method and application.The plant source wide spectrum that the present invention is provided
Antiseptic has the advantages that broad-spectrum antiseptic, gentle, good dissolubility, economy, consumption be small, stable and suitable industrialized production, can be with
Effectively suppress the growth of microorganism in cosmetics, extend the shelf life of cosmetics, while be conducive to ensureing the security of product,
Prevent consumer from being caused possible infection by the product of microorganism pollution because using.The preparation method that the present invention is provided overcomes
Chinese medicine extract smell weight prepared by conventional preparation techniques, active ingredient retains few, and impurity is more, and narrow antimicrobial spectrum, consumption are big, stimulate
The problems such as property is strong.
The present invention adopts the following technical scheme that to solve above-mentioned technical problem：
The invention provides a kind of preparation method of plant source broad spectrum antimicrobial agent, the original of described plant source broad spectrum antimicrobial agent
Material includes material A, water, lipase and pH adjusting agent, is counted using mass fraction as 100 parts, and the material A includes following components：0.1
~5 parts of litsea citrate oil, 0.1~5 part of patchouli oil, 0.1~5 part of citronella oil, 0.1~5 part of hydrolysis ginsenoside and
80~99.6 parts of Miglyol 812N；Described preparation method comprises the following steps：
(1) each component in the material A is well mixed, obtains rich mixture；
(2) water is well mixed with lipase, then adjusts pH value to 7~10, then be well mixed with the rich mixture,
Digested at 40~50 DEG C, accompany by stirring in enzymolysis process, obtain enzymolysis liquid；
(3) it is ultrasonically treated to enzymolysis liquid progress, water-oil separating is then carried out, oil phase is taken；
(4) ripening is carried out to the oil phase, takes supernatant liquid filtering, obtain filtrate, you can.
In the present invention, counted using mass fraction as 100 parts, the material A is preferably comprised following components：0.2~1 part of mountain
Grey seed oil, 0.2~1 part of patchouli oil, 0.2~1 part of citronella oil, 0.2~1 part of hydrolysis ginsenoside and 96~99.2 parts
Miglyol 812N.
Wherein, described litsea citrate oil has this area conventional sense, and it derives from camphorwood section plant, the fruit of cubeb litsen tree
It is real, preferably purchased from Ji'an Guo Guang perfumeries.
Wherein, described patchouli oil has this area conventional sense, and it is from the ground of labiate Pogostemon cablin grass
Upper part, preferably purchased from the perfumery oil Co., Ltd of Ji'an City trillion.
Wherein, described citronella oil has this area conventional sense, and it is from grass family Cymbopogon plants lemon-grass
Herb, preferably purchased from the perfumery oil Co., Ltd of Ji'an City trillion.
Wherein, described hydrolysis ginsenoside has this area conventional sense, and it derives from the root of Araliaceae ginseng
The hydrolysate of ginsenoside in cauline leaf, preferably purchased from Xi'an Cui Yuan bio tech ltd.
Wherein, described Miglyol 812N has this area conventional sense, and it derives from babassu oil palm
Fruit, be palm oil it is refined after derivative, preferably purchased from Shanghai Saifu Chemical Development Co., Ltd..
In the present invention, described water is this area conventional substances, preferably deionized water, the use of described deionized water
Measure as this area conventional amount used, the 1/10~1/5 of the consumption of preferably described material A.
In the present invention, described pH adjusting agent is this area conventional substances, preferably sodium hydroxide, sodium carbonate, carbonic acid
One or more in hydrogen sodium, hydrochloric acid and citric acid.
In step (2), described lipase is this area conventional substances, preferably purchased from the limited public affairs of the outstanding promise biology enzyme in village city
Department；The consumption of described lipase is to adjust the enzymatic activity in solution to the enzymatic activity required for conventional enzyme digestion reaction, preferably
Consumption of the ground for enzymatic activity to be adjusted to the lipase to needed for 10~500u/g, more preferably for enzymatic activity is adjusted to 50~
The consumption of lipase needed for 100u/g.
In step (2), time of described enzymolysis is the conventional enzymolysis time in this area, generally more than 1 hour, preferably
Ground is 1~4 hour.
In step (2), described stirring is this area routine operation, the speed of described stirring is preferably 100~
300rpm, is more preferably 200rpm.
In step (3), described ultrasound is this area routine operation, described ultrasonic frequency is preferably 25000~
35000Hz, is more preferably 30000Hz；The described ultrasonic time is preferably 2~10 minutes.
In step (3), described water-oil separating can be realized using this area routine operation, preferably be stood.It is described
Standing time it is conventional for this area, preferably 0.5~4h.
In step (4), described ageing is this area routine operation, and the temperature of described ageing is preferably -6 DEG C~-2
DEG C, it is more preferably -4 DEG C；The time of described ageing is preferably 8~14 hours, is more preferably 12 hours.
Present invention also offers one kind plant source broad spectrum antimicrobial agent as made from above-mentioned preparation method.
In the present invention, described plant source broad spectrum antimicrobial agent has broad spectrum antibacterial performance, the species of its bacterium that can be resisted compared with
Include the one or more in staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Candida albicans and black-koji mould goodly.
The present invention also provides above-mentioned plant source broad spectrum antimicrobial agent in daily cosmetics and/or external preparation for skin medicine as anti-
The application of rotten agent.
On the basis of common sense in the field is met, above-mentioned each optimum condition can be combined, and produce each preferable reality of the present invention
Example.
Agents useful for same and raw material of the present invention are commercially available.
The positive effect of the present invention is：
(1) present invention makes extract have the work of broad-spectrum antiseptic by the compatibility relationship and synergy between appliable plant
With, and hydrolysis ginsenoside is introduced in the feed, the security of antiseptic is greatly improved；
(2) present invention has incorporated modern biotechnology zymolysis technique in the preparation process of traditional Chinese medicine compound preparation, hence it is evident that reduce
Excitant, substantially increases the antibacterial activity of plant antimicrobial, while improving the influence that bad smell is applied to antiseptic；It is logical
Cross ageing and remove partial impurities, so as to preferably retain small-molecule substance, meeting cosmetics use requirement and aesthetically having weight
Contribute；
(3) whole technical process is all, using vegetable fat and extract as raw material, to prepare under cryogenic in the present invention,
Green natural, energy-conserving and environment-protective；
(4) antiseptic produced by the present invention can be dissolved each other with DPG with arbitrary proportion, because usage amount is relatively low, to weigh
It is convenient, it can be diluted with DPG.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to described reality
Apply among a scope.The experimental method of unreceipted actual conditions in the following example, conventionally and condition, or according to business
Product specification is selected.
In following embodiments, used litsea citrate oil is purchased from Ji'an Guo Guang perfumeries, and patchouli oil is purchased from Ji'an City ten thousand
Hundred million perfumery oil Co., Ltds, citronella oil is purchased from the perfumery oil Co., Ltd of Ji'an City trillion, and hydrolysis ginsenoside extracts source purchased from Xi'an
Bio tech ltd, sad certain herbaceous plants with big flowers acid glycerol three ester is purchased from Shanghai Saifu Chemical Development Co., Ltd., and lipase is purchased from Zaozhuang
The biological Enzyme Co., Ltd of city's outstanding person's promise.
Embodiment 1 (antiseptic)
The preparation method of plant source broad spectrum antimicrobial agent is as follows in the present embodiment：
(1) 0.1g litsea citrate oils, 0.1g patchouli oils, 0.1g citronella oils, 0.1g are hydrolyzed into ginsenoside and 99.6g octanoic acids
Triglyceride DDD is sufficiently mixed uniformly, obtains rich mixture；
(2) 10g deionized waters are taken, lipase is added, are 50u/g to enzymatic activity, pH value is adjusted to 8 using sodium acid carbonate,
It is well mixed with the rich mixture in step (1), is digested under the conditions of 40 DEG C and stirring is accompanied by 2h, enzymolysis process, stirring speed
Rate is 100rpm；
(3) stirring is stopped, ultrasound 2 minutes under the conditions of 30000Hz, then progress water-oil separating in 30 minutes is stood, take oil phase；
(4) oil phase is aged 12 hours at -4 DEG C, takes supernatant liquid filtering, produce the plant source broad spectrum antimicrobial agent.
Embodiment 2 (antiseptic)
The preparation method of plant source broad spectrum antimicrobial agent is as follows in the present embodiment：
(1) 1g litsea citrate oils, 1g patchouli oils, 1g citronella oils, 1g are hydrolyzed into ginsenoside and 96g Caprylic Caprics three
Ester is sufficiently mixed uniformly, obtains rich mixture；
(2) take 10g deionized waters, add lipase, be 100u/g to enzymatic activity, pH value is adjusted to 9 using sodium carbonate, with
Rich mixture in step (1) is well mixed, and is digested under the conditions of 45 DEG C and stirring, stir speed (S.S.) are accompanied by 4h, enzymolysis process
For 200rpm；
(3) stirring is stopped, ultrasound 5 minutes under the conditions of 30000Hz, then 1h progress water-oil separatings are stood, take oil phase；
(4) oil phase is aged 12 hours at -4 DEG C, takes supernatant liquid filtering, produce the plant source broad spectrum antimicrobial agent.
Embodiment 3 (antiseptic)
The preparation method of plant source broad spectrum antimicrobial agent is as follows in the present embodiment：
(1) 5g litsea citrate oils, 5g patchouli oils, 5g citronella oils, 5g are hydrolyzed into ginsenoside and 80g Caprylic Caprics three
Ester is sufficiently mixed uniformly, obtains rich mixture；
(2) take 20g deionized waters, add lipase, be 10u/g to enzymatic activity, using lemon acid for adjusting pH value to 7, with
Rich mixture in step (1) is well mixed, and is digested under the conditions of 50 DEG C and stirring, stir speed (S.S.) are accompanied by 4h, enzymolysis process
For 300rpm；
(3) stirring is stopped, ultrasound 10 minutes under the conditions of 25000Hz, then 4h progress water-oil separatings are stood, take oil phase；
(4) oil phase is aged 8 hours at -6 DEG C, takes supernatant liquid filtering, produce the plant source broad spectrum antimicrobial agent.
Embodiment 4 (antiseptic)
The preparation method of plant source broad spectrum antimicrobial agent is as follows in the present embodiment：
(1) 0.2g litsea citrate oils, 0.2g patchouli oils, 0.2g citronella oils, 0.2g are hydrolyzed into ginsenoside and 99.2g octanoic acids
Triglyceride DDD is sufficiently mixed uniformly, obtains rich mixture；
(2) take 10g deionized waters, add lipase, be 500u/g to enzymatic activity, using sodium hydroxide adjust pH value to
10, it is well mixed with the rich mixture in step (1), is digested under the conditions of 45 DEG C and stirring is accompanied by 4h, enzymolysis process, is stirred
Speed is 200rpm；
(3) stirring is stopped, ultrasound 5 minutes under the conditions of 35000Hz, then 1h progress water-oil separatings are stood, take oil phase；
(4) oil phase is aged 14 hours at -2 DEG C, takes supernatant liquid filtering, produce the plant source broad spectrum antimicrobial agent.
Comparative example 1 (comparative example for not using the antiseptic of biological enzymolysis technology)
The preparation method of antiseptic is as follows in this comparative example：
(1) by 1g litsea citrate oils, 1g patchouli oils, 1g citronella oils, 1g hydrolysis ginsenosides, 96g Caprylic Caprics three
Ester, is sufficiently mixed uniform；
(2) it is aged 12 hours at -10 DEG C, filtering produces the plant source antiseptic agent.
Comparative example 2 (comparative example for being not added with hydrolyzing the antiseptic of ginsenoside in raw material)
The preparation method of antiseptic is as follows in this comparative example：
(1) by 1g litsea citrate oils, 1g patchouli oils, 1g citronella oils, 97g Miglyol 812Ns are sufficiently mixed uniform；
(2) 10g deionized waters are taken, lipase is added, are 100u/g to enzymatic activity, regulation pH value is into 9, with step (1)
Grease mixing, under the conditions of 45 DEG C, stir 4h；
(3) stirring is stopped, under the conditions of 30000 hertz, ultrasound 5 minutes stands 1h, carries out water-oil separating, takes oil phase；
(4) it is aged 12 hours at -10 DEG C, filtering produces the plant source antiseptic agent.
Effect example 1 (bacteriostatic test of antiseptic)
Bacteriostatic test step：
(1) test strain
Staphylococcus aureus (ATCC 8739), Escherichia coli (ATCC 6538), Pseudomonas aeruginosa (ATCC9027), white
Beads coccus (ATCC 10231), black-koji mould (ATCC 16404).
(2) culture medium
TSB solid mediums：Peptone 10g/L, NaCl 10g/L, K2HPO42.5g/L, yeast extract 3g/L, agar
15g/L, distilled water dissolving, regulation pH is 7.2 ± 0.2,115 DEG C of autoclaving 20min；TSB fluid nutrient mediums：Peptone 10g/
L, NaCl 10g/L, K2HPO42.5g/L, yeast extract 3g/L, distilled water dissolving, regulation pH is 7.2 ± 0.2,115 DEG C high
Pressure sterilizing 20min；
SDB solid mediums：Peptone 10g/L, glucose 20g/L, K2HPO43g/L, yeast extract 5g/L, agar
15g/L, distilled water dissolving, 115 DEG C of autoclaving 20min；SDB fluid nutrient mediums：Peptone 10g/L, glucose 20g/L,
K2HPO43g/L, yeast extract 5g/L, distilled water dissolving, 115 DEG C of autoclaving 20min.
(3) bacteria suspension is prepared and is inoculated with
The staphylococcus aureus of glycerol stocks is taken, Escherichia coli, the μ L of Pseudomonas aeruginosa 100 are coated on TSB solid mediums
On, 37 DEG C of culture 2d are resuspended with physiological saline, obtain bacteria suspension, and are counted with plating method, and test bacteria concentration is adjusted to
105~106CFU/mL。
Candida albicanses and the μ L of black-koji mould 100 are coated on SDB solid mediums, 30 DEG C of culture 2d, use physiology salt
Water is resuspended, and obtains bacteria suspension, and is counted with plating method, and test bacteria concentration is adjusted into 105~106。
(4) measure of sample bacteriostasis
Cylinder plate method
Pour into TSB or SDB solid mediums in culture dish, it is to be solidified after, even spread tests bacterium on this culture medium
100μL.It is equidistant on culture medium to put 2 sterile Oxford cup [internal diameter (6.0 ± 0.1) mm, external diameter (8.0 ± 0.1) mm, height
(10.0 ± 0.1) mm, is injected separately into 200 μ L testing samples in cup, with physiological saline or the physiology salt containing a certain amount of DMSO
Water is used as control.In 37 DEG C or 30 DEG C of insulating boxs after culture 2d, the antibacterial circle diameter of various medicines is measured with ruler, takes it to be averaged
Value.
Microdilution plate method
100 μ L testing samples (initial concentration) are added in micropore, the bacteria concentration 1.0 × 10 containing test is added5CFU/mL
For the 2 × TSB or μ L of 2 × SDB fluid nutrient mediums 100, mix, i.e., the test concentrations of testing sample are the 50wt% of initial concentration.
In 30 DEG C or 37 DEG C of insulating boxs after culture 2d, observation has asepsis growth.As a result the premise judged is that growth control is good, blank pair
It is clear according to asepsis growth.
(5) measure of minimum inhibitory concentration (MIC value)
1. minimum suppression staphylococcus aureus concentration (MIC), minimum suppression e. coli concentration (MIC), minimum suppression
Pseudomonas aeruginosa concentration (MIC), the minimum assay method for suppressing candida albicanses concentration (MIC) are as follows：
It is prepared by decoction：By testing sample normal saline dilution into experimental concentration.
It is prepared by bacterium solution：With 2 × TSB or 2 × SDB fluid nutrient mediums dilution bacteria suspension, it is l0 to make its final bacteria concentration5CFU/
mL。
Culture and result interpretation：The μ L of the bacterium solution 100 and μ L of decoction 100 are added in micropore, the negative right of bacterium is not added with while setting
According to be not added with decoction normal growth compare, every kind of medicine do 3 it is parallel, average.Put 37 DEG C or 30 DEG C of wet box are incubated, 48h
After observe result, using direct method read data.As a result the premise judged is that growth control is good, and blank control asepsis growth is clear
Clear, other holes are raised with drug concentration gradient and the growth of bacterium is suppressed.
2. minimum suppression aspergillus niger concentration (MIC) determines
Using cylinder plate method, pour into SDB solid mediums in culture dish, it is to be solidified after, black song is added on this culture medium
Mould (105CFU/ml) 100 μ L, even spread.It is equidistant on culture medium to put 3 sterile Oxford cup [internal diameters (6.0 ± 0.1)
Mm, external diameter (8.0 ± 0.1) mm, height (10.0 ± 0.1) mm, the sample that 200 μ L various concentrations are injected separately into cup (use physiology
Salt solution dilutes).The normal growth control for being not added with test sample and saline control are set simultaneously.As a result the premise judged is growth
Control and saline control well-grown, other with drug concentration gradient rise, the growth of bacterium is suppressed.
The present invention is oily (vegetable oil is diluted to 3% solution with Miglyol 812N) with monotaste plant, and hydrolysis
The issuable known single Miglyol 812 with certain antiseptic effect of process is compared, the antibacterial result of the product such as institute of table 1
Show：
The embodiment of table 1 is compared with the MIC value of monotaste plant oil
As shown in Table 1, within 100 μ L/mL, litsea citrate oil, without antibacterial effect, is read white Escherichia coli, aspergillus niger
Pearl bacterium, Pseudomonas aeruginosa antibacterial effect are general；Within 100 μ L/mL Pogostemon cablin to Pseudomonas aeruginosa without antibacterial effect, to large intestine bar
Bacterium, staphylococcus aureus antibacterial effect are general；Within 100 μ L/mL, citronella oil is to Escherichia coli, Pseudomonas aeruginosa without antibacterial
Effect, it is general to the antibacterial effect of staphylococcus aureus, Candida albicans, aspergillus niger, Capmul MCM C8 to Pseudomonas aeruginosa,
Aspergillus niger antibacterial effect is general, and Capmul MCM C10 is general to Pseudomonas aeruginosa and Candida albicans antibacterial effect.
The antibacterial results contrast of the embodiment of the present invention and comparative example is as shown in table 2：
The embodiment of table 2 is compared with the MIC value of comparative example
The inhibition of 1 pair of each bacterium of comparative example is general as shown in Table 2, and comparative example 2 is antibacterial with embodiment 2
Effect is suitable.
As can be seen here：First, by the reasonable compatibility between plant, the effect of broad-spectrum antiseptic is played；2nd, it is single for each bacterium
From the point of view of solely, the fungistatic effect after compatibility is better than the antibacterial effect of monotaste plant, realizes the result that 1+1 is more than 2, embodies plant
Between synergy on antibacterial effect；3rd, the condensation products after digesting, better than the antibacterial effect of its issuable single component
Really；4th, fungistatic effect can be increased substantially after digesting.
Significantly, the antibiotic effect with wide spectrum, its fungistatic effect is better than simple to the prescription bacteriostasis efficacy of the present invention
Effect, overcomes limitation of the simple to some bacterial strains.Meanwhile, the ratio of three kinds of Chinese medicines of this invention can be to greatest extent
Suppress the growth of bacterium.It is suitable as plant antiseptic agent to use, process program maintains bacteriostasis efficacy, and significantly reduces product
Color, product is stable, is suitable for addition in cosmetics as preservative and uses.
Will be to this hair in technology contents, the objects and the effects of the present invention, the following examples to further illustrate
Bright to be further described, applicant has specially added the collagen and glucose of easy cooperating microorganisms to come effective in embodiment
The using effect of plant antiseptic agent under this technique is said, embodiment does not limit the present invention in any way.All material is quality
Percent concentration.
Embodiment 5 (application of antiseptic prepared by the embodiment of the present invention 1 as preservative in white class product)
The white class product of the present embodiment can be used as moisturiser, repair cream etc., and its composition of raw materials is as follows：
The preparation technology of the white class product of the present embodiment is as follows：
(1) glycerine is taken, in the phase that adds water kettle, Sodium Hyaluronate, Sodium Polyacrylate is added, 300rpm, water intaking and second two is stirred
Amine tetraacethyl disodium is added in the kettle, is heated to temperature for 85 DEG C, is dissolved to clarification, obtains aqueous phase.
(2) taking sad silicic acid triglycerides, docosyl alcohol, VE acetates, EmulgadeSucro, (EmulgadeSucro is business
The name of an article, its specific material is Sucrose Polystearic Acid Esters and Parleam), phytosterol put into oil phase kettle, be heated to temperature
Spend for 85 DEG C, stir as 300rpm, produce oil phase.
(3) (2) oil phase is mixed with (1) aqueous phase in emulsifying kettle, homogeneous (speed is 500rpm) 5min, stirring is cooled to
45℃。
(4) take the embodiment of the present invention 1 to obtain antiseptic, collagen, glucose, 1,2- ethohexadiols to add in (3), stirring speed
Spend for 500rpm, be down to room temperature.
Embodiment 6 (application of antiseptic prepared by the embodiment of the present invention 2 as preservative in white class product)
The white class product of the present embodiment can be used as moisturiser, repair cream etc., and its composition of raw materials is as follows：
The preparation technology of the white class product of the present embodiment is as follows：
(1) glycerine is taken, in the phase that adds water kettle, Sodium Hyaluronate, Sodium Polyacrylate is added, 300rpm, water intaking and second two is stirred
Amine tetraacethyl disodium is added in the kettle, is heated to temperature for 85 DEG C, is dissolved to clarification, obtains aqueous phase.
(2) sad silicic acid triglycerides, docosyl alcohol, VE acetates, EmulgadeSucro, phytosterol is taken to put to oil phase
In kettle, temperature is heated to for 85 DEG C, is stirred as 300rpm, is produced oil phase.
(3) (2) oil phase is mixed with (1) aqueous phase in emulsifying kettle, homogeneous (speed is 500rpm) 5min, stirring is cooled to
45℃。
(4) take the embodiment of the present invention 2 to obtain natural antibacterial agent, collagen, glucose, 1,2- ethohexadiols to add in (3), stir
Speed is mixed for 500rpm, room temperature is down to.
Embodiment 7 (application of antiseptic prepared by the embodiment of the present invention 1 as preservative in water class product)
The water class product of the present embodiment can be used as lotion, moisture retention water, essence lotion etc., and its composition of raw materials is as follows：
The preparation technology of the water class product of the present embodiment is as follows：
(1) glycerine, butanediol are taken, in the phase that adds water kettle, Sodium Hyaluronate is added, 300rpm, water intaking and ethylenediamine tetraacetic is stirred
Acetic acid disodium is added in the kettle, is heated to temperature for 85 DEG C, is dissolved to clarification, obtains aqueous phase.
(2) embodiment of the present invention 1 is taken to obtain natural antibacterial agent, Cremophor RH40,1,2- ethohexadiols, 1,2- pentanediols
In phase of draining the oil kettle, stir, be heated to temperature for 85 DEG C, produce oil phase.
(3) (2) oil phase is added into (1) aqueous phase, quick stirring (speed is 300rpm) 5min, stirring is cooled to 45 DEG C.
(4) collagen and glucose is taken to add in (3), mixing speed is 300rpm, is down to room temperature.
(antiseptic prepared by comparative example 1 of the present invention the answering in white class product as preservative of comparative example 3
With)
The white class product of this comparative example can be used as moisturiser, repair cream etc., and its composition of raw materials is as follows：
The preparation technology of the white class product of this comparative example is as follows：
(1) glycerine is taken, in the phase that adds water kettle, Sodium Hyaluronate, Sodium Polyacrylate is added, 300rpm, water intaking and second two is stirred
Amine tetraacethyl disodium is added in the kettle, is heated to temperature for 85 DEG C, is dissolved to clarification, obtains aqueous phase.
(2) sad silicic acid triglycerides, docosyl alcohol, VE acetates, EmulgadeSucro, phytosterol is taken to put to oil phase
In kettle, temperature is heated to for 85 DEG C, is stirred as 300rpm, is produced oil phase.
(3) (2) oil phase is mixed with (1) aqueous phase in emulsifying kettle, homogeneous (speed is 500rpm) 5min, stirring is cooled to
45℃。
(4) take comparative example 1 of the present invention to obtain natural antibacterial agent, collagen, glucose, 1,2- ethohexadiols to add to (3)
In, mixing speed is 500rpm, is down to room temperature.
(antiseptic prepared by comparative example 2 of the present invention the answering in white class product as preservative of comparative example 4
With)
The white class product of this comparative example can be used as moisturiser, repair cream etc., and its composition of raw materials is as follows：
The preparation technology of the white class product of this comparative example is as follows：
(1) glycerine is taken, in the phase that adds water kettle, Sodium Hyaluronate, Sodium Polyacrylate is added, 300rpm, water intaking and second two is stirred
Amine tetraacethyl disodium is added in the kettle, is heated to temperature for 85 DEG C, is dissolved to clarification, obtains aqueous phase.
(2) sad silicic acid triglycerides, docosyl alcohol, VE acetates, EmulgadeSucro, phytosterol is taken to put to oil phase
In kettle, temperature is heated to for 85 DEG C, is stirred as 300rpm, is produced oil phase.
(3) (2) oil phase is mixed with (1) aqueous phase in emulsifying kettle, homogeneous (speed is 500rpm) 5min, stirring is cooled to
45℃。
(4) take comparative example 2 of the present invention to obtain natural antibacterial agent, collagen, glucose, 1,2- ethohexadiols to add to (3)
In, mixing speed is 500rpm, is down to room temperature.
Comparative example 5 (the conventional water class product in this area)
The water class product of this comparative example can be used as lotion, moisture retention water, essence lotion etc., and its composition of raw materials is such as
Under：
The preparation technology of the water class product of this comparative example is as follows：
(1) glycerine is taken, in the phase that adds water kettle, Sodium Hyaluronate, Sodium Polyacrylate is added, 300rpm, water intaking and second two is stirred
Amine tetraacethyl disodium is added in the kettle, is heated to temperature for 85 DEG C, is dissolved to clarification, obtains aqueous phase.
(2) sad silicic acid triglycerides, docosyl alcohol, VE acetates, EmulgadeSucro, phytosterol is taken to put to oil phase
In kettle, temperature is heated to for 85 DEG C, is stirred as 300rpm, is produced oil phase.
(3) (2) oil phase is mixed with (1) aqueous phase in emulsifying kettle, homogeneous (speed is 500rpm) 5min, stirring is cooled to
45℃。
(4) Capmul MCM C10 of the present invention, collagen, glucose, 1,2- ethohexadiols is taken to add in (3), mixing speed
For 500rpm, room temperature is down to.
Effect example 2 (embodiment 5~7, the experiment of the preservation challenge of comparative example 3~5)
(1) mode and quantity of preservation challenge inoculation：
It is inoculated with using Mixed Microbes.Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa are accessed in testing sample to inoculation
Quantity is 105~106CFU/g or 105~106CFU/ml；It is 10 that candida albicanses and black-koji mould, which are inoculated with quantity,4CFU/g or
104CFU/ml, each three parallel, and blank control is used as using physiological saline.
(2) preservation challenge separation detection
Sample after inoculation is in special time separation detection：0 hour, 7 days, 14 days, 21 days and 28 days.After sampling, according to
Experiment is needed, TSB and SDB culture medium flat plates, 28 DEG C ± 1 DEG C or 36 DEG C ± 1 DEG C are coated on 100 μ L are taken after normal saline dilution
Colony counting after culture.
(3) judgment criteria (according to cosmetics and spices and essence association (CTFA) standard)
It is required that at the 7th day, bacterium reduction by 99.9%, black-koji mould and candida albicanses respectively reduction by 90%, and
Continuous decrease in 28 days, then tested by preservation challenge.
If the average value of any one micro organism quantity in three parallel tests of Mixed Microbes inoculation, at the 7th day at present
Drop to 100CFU/g (CFU/ml) below, 0CFU/g (CFU/ml) or ＜ 10CFU/g (CFU/ml) was all down in 28 days, that
It is considered as antiseptic effect outstanding.
30 hours preservation challenge results of table
4 48 hours preservation challenge results of table
57 days preservation challenge results of table
6 14 days preservation challenge results of table
7 21 days preservation challenge results of table
8 28 days preservation challenge results of table
The preservation challenge result of table 9 collects
Effect example 3 (embodiment 5~7, the human skin patch of comparative example 4)
(1) spot method for testing：Try device from qualified spot, in closed patch test method, by tested material about 0.020g~
0.025g is applied in spot examination device, and external application special adhesive tape is pasted on the bent side of subject's forearm, tested material is removed after 24 hours, in removal
30min after tested material spot examination device, after observing dermoreaction after impression disappearance, is pressed《Cosmetics health specification》Skin in (version in 2007)
Its result of skin reaction packet standard recording.
(2) evaluation of result：Reaction result is recorded by table 10 (skin adverse reaction packet standard), concrete outcome is shown in Table 11.
The skin adverse reaction of table 10 is grouped standard
The embodiment sample of table 11 is to human skin patch result
Conclusion：The human skin patch result of each group is shown：30 subjects skins are in all in 3 embodiments
Negative reaction, and comparative example 4, it is suspicious reaction, only faint erythema (grading system to have 7：0 grade).Foundation《Cosmetics
Hygienic practice》3 groups of embodiments of (version in 2007) human skin patch criterion to human body without skin adverse reaction, it is and right
It is suspicious reaction than embodiment 4, illustrates to add the meaning that hydrolysis ginsenoside is brought in the raw material of the present invention, can greatly improve
The security of preservative.
Claims (10)
1. a kind of preparation method of plant source broad spectrum antimicrobial agent, it is characterised in that the raw material of described plant source broad spectrum antimicrobial agent
Including material A, water, lipase and pH adjusting agent, counted using mass fraction as 100 parts, the material A includes following components：0.1~
5 parts of litsea citrate oil, 0.1~5 part of patchouli oil, 0.1~5 part of citronella oil, 0.1~5 part of hydrolysis ginsenoside and 80
~99.6 parts of Miglyol 812N；Described preparation method comprises the following steps：
(1) each component in the material A is well mixed, obtains rich mixture；
(2) water is well mixed with lipase, regulation pH value is well mixed to 7~10, then with the rich mixture, 40~
Digested at 50 DEG C, accompany by stirring in enzymolysis process, obtain enzymolysis liquid；
(3) it is ultrasonically treated to enzymolysis liquid progress, water-oil separating is then carried out, oil phase is taken；
(4) ripening is carried out to the oil phase, takes supernatant liquid filtering, obtain filtrate, you can.
2. preparation method as claimed in claim 1, it is characterised in that counted using mass fraction as 100 parts, the material A includes
Following components：0.2~1 part of litsea citrate oil, 0.2~1 part of patchouli oil, 0.2~1 part of citronella oil, 0.2~1 part of water
Solve ginsenoside and 96~99.2 parts of Miglyol 812N.
3. preparation method as claimed in claim 1 or 2, it is characterised in that described litsea citrate oil is purchased from Ji'an state light spices
Factory；Described patchouli oil is purchased from the perfumery oil Co., Ltd of Ji'an City trillion；Described citronella oil is purchased from the spices of Ji'an City trillion
Oily Co., Ltd；Described hydrolysis ginsenoside is purchased from Xi'an Cui Yuan bio tech ltd；Described sad certain herbaceous plants with big flowers acid glycerol
Three esters are purchased from Shanghai Saifu Chemical Development Co., Ltd..
4. preparation method as claimed in claim 1, it is characterised in that described water is deionized water, described deionized water
Consumption for the material A consumption 1/10~1/5；Described pH adjusting agent be sodium hydroxide, sodium carbonate, sodium acid carbonate,
One or more in hydrochloric acid and citric acid.
5. preparation method as claimed in claim 1, it is characterised in that in step (2), described lipase is outstanding purchased from Zaozhuang City
Promise biology Enzyme Co., Ltd；Use of the consumption of described lipase for enzymatic activity to be adjusted to the lipase to needed for 10~500u/g
Amount；The time of described enzymolysis is more than 1 hour；The speed of described stirring is 100~300rpm.
6. preparation method as claimed in claim 5, it is characterised in that in step (2), the consumption of described lipase is by enzyme
The consumption of lipase needed for Active Regulation to 50~100u/g；The time of described enzymolysis is 1~4 hour；Described stirring
Speed be 200rpm.
7. preparation method as claimed in claim 1, it is characterised in that in step (3), described ultrasonic frequency is 25000
~35000Hz, the described ultrasonic time is 2~10 minutes；The operation of described water-oil separating is standing；In step (4), institute
The temperature for the ageing stated is -6 DEG C~-2 DEG C, and the time of described ageing is 8~14 hours.
8. preparation method as claimed in claim 7, it is characterised in that in step (3), described ultrasonic frequency is
30000Hz；The time of described standing is 0.5~4h；In step (4), the temperature of described ageing is -4 DEG C, described ageing
Time be 12 hours.
9. plant source broad spectrum antimicrobial agent made from a kind of preparation method as described in claim 1~8 any one.
10. a kind of plant source broad spectrum antimicrobial agent as claimed in claim 9 is made in daily cosmetics and/or external preparation for skin medicine
For the application of preservative.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610169716.3A CN107224408B (en) | 2016-03-23 | 2016-03-23 | Plant-derived broad-spectrum antibacterial agent and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610169716.3A CN107224408B (en) | 2016-03-23 | 2016-03-23 | Plant-derived broad-spectrum antibacterial agent and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107224408A true CN107224408A (en) | 2017-10-03 |
| CN107224408B CN107224408B (en) | 2020-06-02 |
Family
ID=59931524
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610169716.3A Active CN107224408B (en) | 2016-03-23 | 2016-03-23 | Plant-derived broad-spectrum antibacterial agent and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107224408B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101385474A (en) * | 2007-12-27 | 2009-03-18 | 广东省中药研究所 | Plant source natural bactericidal agent |
| CN105076246A (en) * | 2015-08-28 | 2015-11-25 | 无限极（中国）有限公司 | Antibacterial traditional Chinese medicine composition, preparing method of antibacterial traditional Chinese medicine composition and application of antibacterial traditional Chinese medicine composition |
-
2016
- 2016-03-23 CN CN201610169716.3A patent/CN107224408B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101385474A (en) * | 2007-12-27 | 2009-03-18 | 广东省中药研究所 | Plant source natural bactericidal agent |
| CN105076246A (en) * | 2015-08-28 | 2015-11-25 | 无限极（中国）有限公司 | Antibacterial traditional Chinese medicine composition, preparing method of antibacterial traditional Chinese medicine composition and application of antibacterial traditional Chinese medicine composition |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107224408B (en) | 2020-06-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6626902B2 (en) | Antimicrobial herbal composition, method for producing and using the same | |
| CN103432047B (en) | Natural preservative composition and application thereof in cosmetics | |
| CN108143702A (en) | A kind of efficient whitening and moisturizing facial mask liquid, facial mask and preparation method thereof | |
| KR101566320B1 (en) | Cosmetic composition comprising an Impatiens balsamina L, Maca, Rosa multiflora Thunberg, Eryobotrya japonica and Pachyrrhizus erosus Complex-fermented extract | |
| CN105287355B (en) | A kind of U.S. flesh anti-acne essence and preparation method thereof | |
| CN109939064A (en) | The Essence of the metabolite containing probiotics fermention and its application in cosmetics | |
| CN111904909B (en) | Dandruff removing scalp essence containing rose fermentation liquor and preparation method thereof | |
| CN107625690A (en) | Moisten moisturizing camellia oleifera fruit lip gloss and preparation method thereof | |
| CN112516031B (en) | Plant extraction multi-effect composition and preparation method thereof | |
| KR101985381B1 (en) | Cosmetic composition for exfoliating skin keratin comprising fruit fermentation complex made by fermenting grape, orange, apple, lemon and lime | |
| CN108066210A (en) | It is a kind of to utilize ground Folium Camelliae sinensis fermented product of edible mushroom and preparation method and application | |
| CN107058040A (en) | A kind of shaddock vinegar of beautifying face and moistering lotion and its application in cosmetics | |
| CN110974775A (en) | Allergy-relieving composition containing nostoc sphaeroides and preparation method and application thereof | |
| CN105687110A (en) | Plant extract composition for eliminating stretch marks as well as application of composition to cosmetics | |
| JPH01102011A (en) | Skin cosmetic | |
| CN109512736A (en) | A kind of skin care compositions and the cosmetics with careful pore effect | |
| CN107224408A (en) | A kind of plant source broad spectrum antimicrobial agent and its preparation method and application | |
| CN111956546B (en) | Anti-dandruff shampoo containing rose fermentation liquor and preparation method thereof | |
| CN115040442A (en) | Anti-inflammatory toning lotion containing black truffle extract fermentation product and preparation method thereof | |
| CN111789801B (en) | Moisturizing shower gel containing rose fermentation liquor and preparation method thereof | |
| KR20150117436A (en) | Water tissue having the freshness | |
| KR101467162B1 (en) | Essential Composition with Carboxy Generating Substance for Improving Blood Flow and Treating Acne and Method for Producing the Same | |
| CN113244140A (en) | Composition for regulating skin micro-ecological balance and application and preparation method thereof | |
| CN109806205A (en) | A kind of FRUCTUS TERMINALIAE IMMATURUS extract and its antibacterial application | |
| KR102520908B1 (en) | Preparation of aged solution of fruit of dioscorea opposita thumb, and aged solution of fruit of dioscorea opposita thumb prepared thereby |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 201404 workshop 1, building 4, No. 666, Jinbi Road, Jinhui Town, Fengxian District, Shanghai Patentee after: Shanghai Zhina Biotechnology Co.,Ltd. Patentee after: LAIBO COSMETICS TECHNOLOGY (SHANGHAI) Co.,Ltd. Address before: 201405 room 1237, building 15, 1999 Guangtai Road, Fengxian District, Shanghai Patentee before: SHANGHAI SHENGWEI BIOLOGICAL TECHNOLOGY Co.,Ltd. Patentee before: LAIBO COSMETICS TECHNOLOGY (SHANGHAI) Co.,Ltd. |
|
| CP03 | Change of name, title or address |