A kind of bath foam and preparation method thereof containing natural bacteriostatic active constituent
Technical field
The present invention relates to daily use chemicals technical fields, and in particular to a kind of bath foam and its system containing natural bacteriostatic active constituent
Preparation Method.
Background technology
Shower cream is the cleaning product for cleaning and moisturizing the skin made of surfactant and conditioner modulation, existing
The necessity for life of modern is had become, moreover, with the continuous improvement of living standards, demand of the people to shower cream is also got over
Come bigger, the type of shower cream is more and more therewith, so requirement of the people to the quality and effect of bath article is also increasingly
Height, therefore the bath article with natural nutrient component is obtained for the welcome of consumer mostly in the market.But it is existing natural
The clean effect of auxotype bath article is not strong, has a single function, and formula is complicated.
Oil tea system Theaceae Camellia Plants, evergreen dungarunga are the distinctive seeds in China, are concentrated mainly on Zhejiang, river
West, Henan, Hunan, Guang Xiwu are saved.57,500,000 mu are had reached to 2013 end of the year China's camellia oleifera lam total cultivated areas, produces tea seed per year
Up to more than 760,000 tons, generally 90% or more, be one kind has unsaturated fatty acid content in the tea-seed oil produced using tea seed
The table oil of healthcare function.And tea seed extract oil when will produce about 60% tea seed cake, camellia seed meal contain there are many it is useful at
Divide crude protein, crude fat, carbohydrate, crude fibre, Tea Saponin 10-14%, tannin, caffeine etc..The reasonable development profit of camellia seed meal
With being camellia oleiferaindustry researcher all very concerns, and camellia seed meal is not utilized well at present, mostly directly
Make pool-cleaning agent, fuel use, causes the prodigious wasting of resources, therefore the utilization of camellia seed meal resource are urgently to be resolved hurrily.Closely
Nian Lai has increasingly caused the utilization of tea cake the great attention of various regions, as the extraction process of tea seed cake is obtained into one
Step exploitation, tea seed cake will be developed and used further.
Oil tea extract be rich in active skull cap components Tea Saponin, Tea Saponin is a kind of three mushroom class compound of five rings, by sugared body,
Glucoside member and organic acid composition, it is a kind of natural nonionic surface active agent, has and disperses, emulsifies, foaming, moistening, oozing
Saturating isoreactivity effect, it is small to be formed by emulsion particle, is evenly distributed, stability is good.Meanwhile it can significantly decrease the table of water
Face tension, and there is fine stability in hard water;Tea Saponin has very strong foamability, and Tea Saponin property is mild, right
Skin irritation is small, without apparent malicious rational role;Tea Saponin possesses highly significant fungistatic effect, and Tea Saponin can be used as matrix
Ingredient is in the washing products such as shampoo, bath foam, hand cleanser.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of bath foam and its system containing natural bacteriostatic active constituent
Preparation Method.
In a first aspect, the present invention provides a kind of bath foams containing natural bacteriostatic active constituent, by weight percentage,
Including:
Wherein, the oil tea bacteriostatic extractive is at least one of compound P1 and P2, the chemical constitution of compound P1
Formula is as shown in formula I:
The chemical constitution of P2 is as shown in formula II:
Preferably, the chelating agent is disodium ethylene diamine tetraacetate (EDTA-2Na) and tetrasodium ethylenediamine tetraacetate (EDTA-
At least one of 4Na).
It is further preferred that the chelating agent is EDTA-2Na.
Preferably, the skin conditioner is at least one of ethylene glycol, glycerine and lanolin.
It is further preferred that the skin conditioner is glycerine and lanolin.
Preferably, the thickener is at least one of ammonium chloride, hydroxyethyl cellulose and sodium chloride.
It is further preferred that the thickener is hydroxyethyl cellulose.
Preferably, the pH adjusting agent is sodium hydroxide.
Preferably, in the bath foam containing natural bacteriostatic active constituent, the weight hundred of the oil tea bacteriostatic extractive
Divide than being 0.05-2% or 0.05%-1%.
Preferably, the bath foam containing natural bacteriostatic active constituent further includes by weight percentage frosting agent
0.01-1%.
It is further preferred that the frosting agent is tea seed cake powder, the tea seed cake powder is preferably sized to 20-200 mesh.
It is understood that tea seed cake powder is as the pure natural frosted particle in taking a shower as described in the present invention, when in use,
The coarse keratinized tissue and pore dirt of body surface can be removed by the tea seed cake powder of suspension, and small to the irritation of skin, can be used as
Granule for massage is effectively facilitated blood circulation, and relaxed muscle alleviates the biotonus caused by operating pressure, is suitble to length
Phase uses.
Second aspect, the present invention provides a kind of preparation methods of the bath foam containing natural bacteriostatic active constituent, including
Following steps:
(1) by sodium sulfate of polyethenoxy ether of fatty alcohol (AESA), cocoanut fatty acid diethanolamide (6501), cocounut oil acyl
Amine propyl betaine (CAB-35), oil tea extract, skin conditioner are soluble in water, are uniformly mixed.
(2) mixture obtained by step (1) is heated to 60-80 DEG C (preferably 70 DEG C), lauryl sodium sulfate is added
(K12), chelating agent, thickener, make it dissolve, and are uniformly mixed, it is then cooled to room temperature.
(3) it uses pH adjusting agent that the pH value of mixture obtained by step (2) is adjusted to 5.0-6.0, obtains antibacterial containing oil tea
The bath foam of substance.
According to the bath foam containing natural bacteriostatic active constituent obtained by above-mentioned steps, by weight percentage, including:
Wherein, the oil tea bacteriostatic extractive is at least one of compound P1 and P2, the chemical constitution of compound P1
Formula is as shown in formula I:
The chemical constitution of P2 is as shown in formula II:
Preferably, the chelating agent is at least one of EDTA-2Na and EDTA-4Na.
It is further preferred that the chelating agent is EDTA-2Na.
Preferably, the skin conditioner is at least one of ethylene glycol, glycerine and lanolin.
It is further preferred that the skin conditioner is glycerine and lanolin.
Preferably, the thickener is at least one of ammonium chloride, hydroxyethyl cellulose and sodium chloride.
It is further preferred that the thickener is hydroxyethyl cellulose.
Preferably, the pH adjusting agent is sodium hydroxide.
Preferably, in the step (2), further include:
Mixture obtained by step (1) is added in tea seed cake powder, is stirred;Wherein, tea seed cake powder, which accounts for, described contains natural bacteriostatic
The weight percent of the bath foam of active constituent is 0.01-1%.
It is further preferred that the tea seed cake powder is obtained by the finely ground sieving of tea seed cake raw material.
It is understood that any one skilled in the art can be by provided by the invention containing natural
Formula of bath foam of bacteriostatic active ingredients and preparation method thereof is prepared for production in the washing products such as shampoo, hand cleanser.
The beneficial effects of the present invention are:
(1) present invention is had compared with the formula of existing bath product using the natural bacteriostatic active constituent extracted in tea seed cake
There is antibacterial, anti-oxidant, sun-proof anti-purple, moisturizing and other effects;And stronger dirt-removing power and foamability are had both, it can replace
Other chemical substances, to no damage to human body;
(2) present invention uses natural tea seed cake powder as pure natural frosted particle in bath foam, when in use, can be by outstanding
The coarse keratinized tissue and pore dirt of floating tea seed cake powder removal body surface, and it is small to the irritation of skin, it is alternatively arranged as massage
Grain is effectively facilitated blood circulation, and relaxed muscle alleviates the biotonus caused by operating pressure, is suitble to be used for a long time;
(3) present invention is that new approach is found in tea seed cake comprehensive utilization, can largely utilize tea seed cake raw material well, effectively keep away
Exempt from the waste of tea seed cake, there is higher social benefit.
Specific implementation mode
With reference to embodiment, the present invention will be further described.
Embodiment 1
A kind of preparation method of oil tea bacteriostatic extractive, includes the following steps:
(1) feedstock processing:Tea seed cake is crushed to 20-80 mesh, obtains tea powder raw material.
(2) continuous phase transistion extracts:It by tea powder raw material 1.5kg obtained by step (1) and is fitted into extraction kettle, extracts being consistently lower than
Under conditions of taking critical pressure and the critical-temperature of agent, by a concentration of 80% ethyl alcohol extractant boil down to liquid, in extraction temperature
Under conditions of 80 DEG C of degree, extracting pressure 0.4MPa, extraction kettle is flowed through with the flow velocity of 100L/h, continuous extraction 1h is extracted in oil tea
After antibacterial substance, under conditions of 80 DEG C of resolution temperature, parsing pressure 0.2MPa, flows through in extraction-container, obtain extract 303g.
(3) after being concentrated and dried the antibacterial substance obtained by step (2), distillation water dissolution is added, shakes up, is transferred to separatory funnel
In, the petroleum ether of 4 times of volumes is added, shake well extraction is stood, and after solution completely layering, releases the petroleum ether extraction on upper layer
Liquid is taken, petroleum ether extract is concentrated under reduced pressure to obtain.
(4) after distillation water dissolution being added in petroleum ether extract obtained by step (3), the ethyl acetate of 4 times of volumes is added, fills
Divide shaking out, stand, after solution completely layering, releases the acetic acid ethyl acetate extract on upper layer, ethyl acetate is concentrated under reduced pressure to obtain
Extract.
(5) after distillation water dissolution being added in acetic acid ethyl ester extract obtained by step (4), the n-butanol of 4 times of volumes is added, fills
Divide shaking out, stand, after solution completely layering, releases the butanol extraction liquid on upper layer, until n-butanol layer clear, colorless,
Extract liquor is merged, n-butyl alcohol extract is concentrated under reduced pressure to obtain.
(6) after being concentrated and dried the middle gained n-butyl alcohol extract of step (5), using high speed adverse current chromatogram (HSCCC) to institute
N-butyl alcohol extract is obtained to be isolated and purified;The condition of high speed adverse current chromatogram (HSCCC) is that ethyl acetate-n-butanol-water (contains
3% acetic acid) (1:4:4, V/V) system, flow velocity 1.5ml/min, rotating speed 850r/min, sample size 500ml are into sample liquid
3ml collects the corresponding component in three peaks, is respectively designated as F1, F2 (P1), F3, concentrated freeze-dried object P1, the weight of P1 is respectively
50g, purity 98.5% are spare.
Oil tea extract P1 is Kaempferol -3-O- { β-D- glucopyranoses-(1 → 2)-[α-L- rhamnoses-(1 → 6)] -
β-D-Glucose glucoside } (i.e. aempferol-3-O- { β-D-glucopyranosyl- (1 → 2)-[α-L-
Rhamnopyranosyl- (1 → 6)]-β-D-glucopyranoside }), chemical structural formula is as shown in formula I:
For the advantageous effect further illustrated the present invention, above-mentioned experimental procedure is repeated, by the F3 components of gained using efficient
Liquid chromatogram (HPLC) further detaches, HPLC operating conditions:Composing column selects C18 chromatographic columns, mobile phase to select 30% methanol
Solution, Detection wavelength 210nm, flow velocity 10ml/min, sample size are 50 μ l, sample concentration 15mg/ml;It is obtained after freeze-drying
The weight of P2, P2 are 50g, and purity 98.7% is spare.
The oil tea extract P2 be Kaempferol -3-O- β-D- xylopyranoses-(1 → 2)-[α-L- rhamnoses-(1 →
6)]-β-D-Glucoses glucoside } (kaempferol-3-O- { β-D-xylopyranosyl- (1 → 2)-[α-L-
Rhamnopyranosyl- (1 → 6)]-β-D-glucopyranoside }), chemical constitution is as shown in formula II:
Embodiment 2
(1) a kind of preparation method of the bath foam containing oil tea bacteriostatic extractive, includes the following steps:
1. by sodium sulfate of polyethenoxy ether of fatty alcohol (AESA), cocoanut fatty acid diethanolamide (6501), cocounut oil acyl
Oil tea antibacterial substance, the glycerine that amine propyl betaine (CAB-35), embodiment 1 provide are soluble in water, are uniformly mixed.
2. mixture obtained by step (1) is heated to 70 DEG C, lauryl sodium sulfate (K12), EDTA-2Na, hydroxyl second is added
Base cellulose, makes it dissolve, and is uniformly mixed, it is then cooled to room temperature.
3. the pH value of mixture obtained by step (2) is adjusted to 6.0 with sodium hydroxide, acquisition contains oil tea bacteriostatic extractive
Bath foam;Wherein, by weight percentage, by sodium sulfate of polyethenoxy ether of fatty alcohol (AESA), lauryl sodium sulfate
(K12), cocoanut fatty acid diethanolamide (6501), Cocoamidopropyl betaine (CAB-35), EDTA-2Na, water solubility
Lanolin, glycerine, hydroxyethyl cellulose are fixed to 13%, 6%, 3%, 5%, 0.1%, 2%, 2%, 1.3%;Oil tea
The content of bacteriostatic extractive is as shown in table 1.
The content of compound P1 and P2 in bath foam of the table 1 containing oil tea bacteriostatic extractive
(2) according to extraordinary bath agent standard GB/T 19877.2 and the Ministry of Public Health《Disinfection technology standard》, with the following method
Detect fungistatic effect:
1. Spawn incubation
Escherichia coli are cultivated:The strain Escherichia coli of picking slant preservation is forwarded to equipped with 10ml nutrient broth Liquid Cultures
In the test tube of base, 37 DEG C of stationary culture 48-72h.
Staphylococcus aureus is cultivated:The staphylococcus aureus kind of picking slant preservation is forwarded to equipped with 10ml nutrient meats
In the test tube of soup fluid nutrient medium, 37 DEG C of stationary culture 18-24h.
2. bacteria suspension:Staphylococcus aureus or Escherichia coli fresh cultured object for 24 hours are taken, with the phosphorus of peptone containing 1000mg/L
Phthalate buffer rinses lower culture, is configured to required 1 × 105The bacteria suspension of cfu/ml is spare.
3. test group:The bath foam sample of the oil tea bacteriostatic extractive as shown in table 1 containing various concentration is made respectively
50mm × 50mm size prints are put in sterile vessel piecewise after 75% ethanol disinfection, and 1.0ml experiments is taken to be dripped with bacteria suspension
Contaminate in print center, smoothen, make bacterium solution and print edge there are 5mm at a distance from, set and dry 30min in 37 DEG C of incubators, as dye
The antibacterial print of bacterium is spare;There is bacterium smooth in sterile letheen planar surface up the antibacterial print of microbiological contamination;With semisolid fine jade
Fat 5.0ml, uniform fold is in microbiological contamination sample surface, and setting culture in 37 DEG C of incubators, for 24 hours, observation is as a result, experiment is repeated 3 times.
4. control group:Repeat the above steps 3., by step 3. in oil tea bacteriostatic extractive containing various concentration wash one's hair
Bath foam sample is substituted for existing formula shower cream (according to embodiment 1 in the patent document of Patent No. CN 201310599343.X
The step of prepared shower cream), commercially available product Australia avenge shower cream, experiment is repeated 3 times.
5. blank control group:Experiment bacteria suspension is made into appropriate dilution, make its a concentration of 1 × 103Cfu/ml takes it
0.1ml drops dye is smoothened on the homogeneity print of the bath foam without oil tea antibacterial substance, after doing same processing with test group print,
With putting in a tablet, is covered and cultivated with semi-solid agar, as positive control;Simultaneously, experiment bacteria suspension is as viable bacteria meter for experiment
Number, and the culture for observing the control tested bacterium of print without oil tea antibacterial substance counts, experiment is repeated 3 times.
The calculating of bacteriostasis rate:Bacteriostasis rate=[(control average colony number-experiment average colony number)/control average colony number]
× 100%.
(3) malicious combability measurements
The healthy mice 80 of weight 20-25g, half male and half female is selected to be divided into 12 groups, including ten groups of test groups,
It is divided into the 2-3 bath foam for giving the clear water that accumulated dose is 20g/kg and the oil tea antibacterial substance containing various concentration in for 24 hours, adopts
Intragastrically is inserted into white mouse stomach with syringe and is injected, and observes white mouse death condition.
(4) recruitment evaluation
600 volunteers are chosen, are divided into 12 groups, every group of 50 people, volunteer is to the oil tea containing various concentration
The bath oil of antibacterial substance is tried out, 30 days trial periods, and the oil tea containing various concentration is antibacterial in use (1) respectively weekly carries
The bath foam, existing formula shower cream and commercially available product Australia of object is taken to avenge shower cream 2-3 times;Subject is collected to detergency performance, skin
The evaluation of pleasant sense project, effective percentage=efficiently individual quantity/tested number × 100% after the inhibition of skin itch, bath.
Test result
(1) fungistatic effect is tested:The bacteriostatic test result of the bath foam of oil tea bacteriostatic extractive containing various concentration is such as
Shown in table 2, wherein 1-9 groups correspond to the bath foam of the oil tea bacteriostatic extractive of various concentration in table 1 respectively.The result shows that containing
The bath foam of bacteriostatic compound is to the bacteriostasis rate of Escherichia coli and staphylococcus aureus 99% or more, wherein oil tea presses down
In the concentration range of a concentration of 0.05-2% of fungus extract, the bath foam containing 0.1% compound P1 and 0.1% compound P1
Fungistatic effect it is best.
The bacteriostatic test result of the different bath foams of table 2
(2) malicious combability measurements:The toxicity test result of the bath foam of oil tea bacteriostatic extractive containing various concentration is aobvious
Show:It is observed continuously seven days, none is dead for small white mouse, and has no abnormal symptom.Test result shows containing the antibacterial of various concentration
Median lethal dose LD of the bath foam of compound to male and female small white mouse50It is all higher than 20g/kg, the true nontoxic grade in border.
(3) recruitment evaluation:The recruitment evaluation of different bath foams is as shown in table 3, with existing formula shower cream and commercially available product
Australia's snow shower cream is compared, and the detergency of the bath foam containing bacteriostatic compound P1 and/or P2 is strong, foaming abundancy, and antipruritic effect is bright
Aobvious, dermal sensation is pleasant after bathing, wherein with the bath foam (the 4th group) containing 0.1% compound P1 and 0.1% compound P2
Comprehensive performance it is best.
The recruitment evaluation of the different bath foams of table 3
Embodiment 3
The step of the step of advantageous effect in order to further illustrate the present invention, repetition embodiment 2 (1), repetition embodiment 2
(1), it is additionally added tea seed cake powder in step (1), obtains the bath foam A containing oil tea bacteriostatic extractive and tea seed cake powder, bath foam B
And bath foam C, wherein each component and its weight percent are as shown in table 4.
Each component and its content in 4 bath foam of table
According to (2)-(4) the step of embodiment 2, above-mentioned three kinds of bath foams are subjected to fungistatic effect experiment, malicious combability measurements
And recruitment evaluation.
Test result
(1) fungistatic effect is tested:The bacteriostatic test result of the bath foam of oil tea antibacterial substance containing various concentration such as table 5
It is shown,
The bacteriostatic test result of the different bath foams of table 5
(2) malicious combability measurements:The toxicity test result of the bath foam of oil tea antibacterial substance containing various concentration is shown:
It is observed continuously seven days, none is dead for small white mouse, and has no abnormal symptom.Test result shows that the oil tea containing various concentration is antibacterial
Median lethal dose LD of the bath foam of substance to male and female small white mouse50It is all higher than 20g/kg, the true nontoxic grade in border.
(3) recruitment evaluation:The results are shown in Table 6 for the recruitment evaluation of different bath foams, and three kinds antibacterial containing tea seed cake powder, oil tea
The bath foam of extract all has that detergency is strong, antipruritic effect is apparent, the pleasant feature of dermal sensation after bathing;Wherein, to wash one's hair
The comprehensive performance of bath foam A (containing 0.05% tea seed cake powder) is best.
The recruitment evaluation of the different bath foams of table 6
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.