CN105287301A

CN105287301A - Bath liquid containing camellia seed cake extract and preparation method thereof

Info

Publication number: CN105287301A
Application number: CN201510828113.5A
Authority: CN
Inventors: 丘苑新; 赵丽; 潘婷; 柳建良
Original assignee: Zhongkai University of Agriculture and Engineering
Current assignee: Zhao Xianliang
Priority date: 2015-11-24
Filing date: 2015-11-24
Publication date: 2016-02-03
Anticipated expiration: 2035-11-24
Also published as: CN105287301B

Abstract

The invention provides a bath liquid containing natural components with bacteriostatic activity and a preparation method thereof. Compared with the formula of a bath product in the prior art, the bath liquid is rich in natural components with bacteriostatic activity, and has bacteriostasis, antioxidation, sun protection, UV protection, moisture retention, moistening and other efficacies; the bath liquid has good cleaning and foaming capabilities, can replace other chemical substances, and does not harm human body; natural camellia seed cake powder is used, and can be used as pure natural scrubbing particles in the bath liquid for removing rough keratinized tissues and dirt in pores on the body surface; the natural camellia seed cake powder can be used as massage particles for effectively promoting blood circulation, relaxing muscle, alleviating mental stress due to work pressure, and is suitable for long-term usage; furthermore, the preparation method is simple and highly efficient, and provides a new approach for integrated utilization of the camellia seed cake; the method has highly economic and social benefits.

Description

A kind of bath foam containing the withered extract of tea and preparation method thereof

Technical field

The present invention relates to daily use chemicals technical field, be specifically related to a kind of bath foam containing natural bacteriostatic active component and preparation method thereof.

Background technology

Bath gel be by surfactant and conditioner modulate for cleaning product that is clean and skin care, now become the necessity for life of modern, and, along with improving constantly of living standard, people are also just increasing to the demand of bath gel, the kind of bath gel gets more and more thereupon, thus people to the quality of bath article and the requirement of effect also more and more higher, therefore bath article market with natural nutrient component is obtained for the welcome of consumer mostly.But the clean effect of existing native trophism bath article is not strong, and function singleness, formula is complicated.

Oil tea system Theaceae Camellia Plants, evergreen dungarunga is the distinctive seeds of China, mainly concentrates on Zhejiang, Jiangxi, Henan, Hunan, Guang Xiwu province.To 2013 the end of the year China's camellia oleifera lam total cultivated area reached 5,750 ten thousand mu, produce per year Semen Camelliae reach more than 760,000 tons, in the Oleum Camelliae utilizing Semen Camelliae to produce, unsaturated fatty acid content is generally more than 90%, is a kind of table oil with health care.And Semen Camelliae oil expression time can produce about 60% tea withered, camellia seed meal contains multiple useful component crude protein, crude fat, saccharide, crude fibre, tea saponin 10-14%, tannin, caffeine etc.The rational exploitation and utilization of camellia seed meal is the problem that camellia oleiferaindustry researcher is all extremely concerned about, and camellia seed meal is not well utilized at present, mostly directly make pool-cleaning agent, fuel uses, cause the very large wasting of resources, therefore the exploitation of camellia seed meal resource are urgently to be resolved hurrily.In recent years, the exploitation of CHAKUBING are caused day by day to the great attention of various places, the extraction process withered along with tea is developed further, and tea is withered will further be developed.

Oil tea extract is rich in active skull cap components tea saponin, tea saponin is a kind of five rings three mushrooms compound, be made up of sugared body, glycoside unit and organic acid, it is a kind of natural nonionic surfactant, there is dispersion, emulsifying, foaming, moistening, infiltration isoreactivity effect, the emulsion particle formed is little, is evenly distributed, good stability.Meanwhile, it can reduce the surface tension of water significantly, and has fine stability in hard water; Tea saponin has very strong foamability, and tea saponin character is gentle, little to skin irritation, without obvious malicious rational role; Tea saponin has extremely significant fungistatic effect, and tea saponin can be used in the washing products such as shampoo, bath foam, handwashing liquid as matrix components.

Summary of the invention

For the deficiencies in the prior art, the invention provides a kind of bath foam containing natural bacteriostatic active component and preparation method thereof.

First aspect, the invention provides a kind of bath foam containing natural bacteriostatic active component, by weight percentage, comprising:

Wherein, described oil tea bacteriostatic extractive is at least one in compound P1 and P2, and the chemical structural formula of compound P1 is as shown in formula I:

The chemical constitution of P2 is as shown in formula II:

Preferably, described chelating agen is at least one in disodiumedetate (EDTA-2Na) and tetrasodium ethylenediamine tetraacetate (EDTA-4Na).

Further preferably, described chelating agen is EDTA-2Na.

Preferably, described skin protectant is at least one in ethylene glycol, glycerol and lanoline.

Further preferably, described skin protectant is glycerol and lanoline.

Preferably, described thickening agent is at least one in ammonium chloride, hydroxyethyl-cellulose and sodium chloride.

Further preferably, described thickening agent is hydroxyethyl-cellulose.

Preferably, described pH adjusting agent is sodium hydroxide.

Preferably, described containing in the bath foam of natural bacteriostatic active component, the percentage by weight of described bacteriostatic compound is 0.05-2% or 0.05%-1%.

Preferably, the described bath foam containing natural bacteriostatic active component, by weight percentage, also comprises frosting agent 0.01-1%.

Further preferably, described frosting agent is the withered powder of tea, and the size of the withered powder of described tea is preferably 20-200 order.

Be understandable that, the withered powder of tea as described in the present invention is as the pure natural frosted granule in shower, in use, the withered powder of tea by suspending removes coarse keratinized tissue and the pore dirt of body surface, and little to the zest of skin, can be used as granule for massage, blood circulation promoting effectively, relaxed muscle, alleviates the biotonus because operating pressure causes, and is applicable to life-time service.

Second aspect, the invention provides a kind of preparation method of the bath foam containing natural bacteriostatic active component, comprises the steps:

(1) polyoxyethylenated alcohol sodium sulfate (AESA), cocoanut fatty acid diethanolamide (6501), cocamido propyl betaine (CAB-35), oil tea extract, skin protectant is soluble in water, mix homogeneously.

(2) step (1) gained mixture is heated to 60-80 DEG C (being preferably 70 DEG C), adds sodium lauryl sulphate (K12), chelating agen, thickening agent, make it dissolve, and mix homogeneously, then, be cooled to room temperature.

(3) adopt pH adjusting agent that the pH value of step (2) gained mixture is adjusted to 5.0-6.0, obtain the bath foam containing oil tea antibacterial substance.

According to the bath foam containing natural bacteriostatic active component of above-mentioned steps gained, by weight percentage, comprising:

The chemical constitution of P2 is as shown in formula II:

Preferably, described chelating agen is at least one in EDTA-2Na and EDTA-4Na.

Further preferably, described chelating agen is EDTA-2Na.

Further preferably, described skin protectant is glycerol and lanoline.

Further preferably, described thickening agent is hydroxyethyl-cellulose.

Preferably, described pH adjusting agent is sodium hydroxide.

Preferably, in described step (2), also comprise:

Withered for tea powder is added step (1) gained mixture, is uniformly mixed; Wherein, the withered powder of tea accounts for the percentage by weight of the described handwashing liquid containing the withered extract of tea is 0.01-1%.

Further preferably, the withered powder of described tea to be sieved acquisition by the withered raw material porphyrize of tea.

Be understandable that, any those skilled in the art of being familiar with can by formula of the bath foam containing natural bacteriostatic active component provided by the invention and preparation method thereof for the production of preparing in the washing product such as shampoo, handwashing liquid.

Beneficial effect of the present invention is:

(1) the present invention is compared with the formula of existing bath product, uses the natural bacteriostatic active component of tea withered middle extraction to have the effects such as antibacterial, antioxidation, sun-proof anti-purple, moisturizing; And have stronger dirt-removing power and foamability concurrently, other chemical substances can be replaced, to human body fanout free region;

(2) the present invention adopts the withered powder of natural tea as pure natural frosted granule in bath foam, in use, the withered powder of tea by suspending removes coarse keratinized tissue and the pore dirt of body surface, and it is little to the zest of skin, also can be used as granule for massage, effectively blood circulation promoting, relaxed muscle, alleviate the biotonus because operating pressure causes, be applicable to life-time service;

(3) the present invention is that new approach is found in the withered comprehensive utilization of tea, can utilize the withered raw material of tea well in a large number, effectively avoid the waste that tea is withered, have higher social benefit.

Detailed description of the invention

Below in conjunction with embodiment, the present invention will be further described.

Embodiment 1

A preparation method for oil tea bacteriostatic extractive, comprises the steps:

(1) Feedstock treating: be crushed to 20-80 order by withered for tea, obtain tea powder raw material.

(2) continuous phase transistion extraction: step (1) gained tea powder raw material 1.5kg is loaded in extraction kettle, all the time lower than under the critical pressure of extractant and the condition of critical temperature, be the alcohol extraction agent boil down to liquid of 80% by concentration, under the condition of extraction temperature 80 DEG C, extracting pressure 0.4MPa, extraction kettle is flowed through with the flow velocity of 100L/h, continuous extraction 1h, in extraction oil tea after antibacterial substance, under the condition of resolution temperature 80 DEG C, parsing pressure 0.2MPa, flow through in extraction-container, obtain extract 303g.

(3) by after the antibacterial substance concentrate drying of step (2) gained, add distilled water to dissolve, shake up, proceed in separatory funnel, add the petroleum ether of 4 times of volumes, shake well extracts, leave standstill, after the complete layering of solution, release the petroleum ether extraction liquid on upper strata, concentrating under reduced pressure obtains petroleum ether extract.

(4) after step (3) gained petroleum ether extract being added distilled water dissolving, add the ethyl acetate of 4 times of volumes, shake well extracts, leave standstill, after the complete layering of solution, release the acetic acid ethyl acetate extract on upper strata, concentrating under reduced pressure obtains acetic acid ethyl ester extract.

(5) after step (4) gained acetic acid ethyl ester extract being added distilled water dissolving, add the n-butyl alcohol of 4 times of volumes, shake well extracts, leave standstill, after the complete layering of solution, release the butanol extraction liquid on upper strata, until n-butanol layer clear, colorless, merged by extract, concentrating under reduced pressure obtains n-butyl alcohol extract.

(6) by after gained n-butyl alcohol extract concentrate drying in step (5), high speed adverse current chromatogram (HSCCC) is adopted to carry out separation and purification to gained n-butyl alcohol extract; The condition of high speed adverse current chromatogram (HSCCC) is ethyl acetate-n-butanol-water (containing 3% acetic acid) (1:4:4, V/V) system, and flow velocity is 1.5ml/min, rotating speed is 850r/min, and sample size is 500ml, and sample introduction liquid is 3ml, collect component corresponding to three peaks respectively, called after F1 respectively, F2 (P1), F3, concentrated freeze-dried thing P1, the weight of P1 is 50g, and purity is 98.5%, for subsequent use.

Oil tea extract P1 is kaempferol-3-O-{ β-D-Glucopyranose .-(1 → 2)-[α-L-rhamnose-(1 → 6)]-β-D-Glucose glycoside } (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 further illustrating beneficial effect of the present invention, repeat above-mentioned experimental procedure, high performance liquid chromatography (HPLC) is adopted to be separated further the F3 component of gained, HPLC operating condition: C18 chromatographic column selected by spectrum post, mobile phase selects the methanol solution of 30%, and determined wavelength is 210nm, flow velocity 10ml/min, sample size is 50 μ l, sample concentration 15mg/ml; Obtain P2 after lyophilization, the weight of P2 is 50g, and purity is 98.7%, for subsequent use.

Described oil tea extract P2 is kaempferol-3-O-{ β-D-xylopyranose-(1 → 2)-[α-L-rhamnose-(1 → 6)]-β-D-Glucose glycoside } (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) preparation method for the bath foam containing oil tea bacteriostatic extractive, comprises the steps:

1. oil tea antibacterial substance polyoxyethylenated alcohol sodium sulfate (AESA), cocoanut fatty acid diethanolamide (6501), cocamido propyl betaine (CAB-35), embodiment 1 provided, glycerol are soluble in water, mix homogeneously.

2. step (1) gained mixture is heated to 70 DEG C, adds sodium lauryl sulphate (K12), EDTA-2Na, hydroxyethyl-cellulose, make it dissolve, and mix homogeneously, then, be cooled to room temperature.

3. with sodium hydroxide, the pH value of step (2) gained mixture is adjusted to 6.0, obtains the bath foam containing oil tea bacteriostatic extractive; Wherein, by weight percentage, polyoxyethylenated alcohol sodium sulfate (AESA), sodium lauryl sulphate (K12), cocoanut fatty acid diethanolamide (6501), cocamido propyl betaine (CAB-35), EDTA-2Na, water solublity lanoline, glycerol, hydroxyethyl-cellulose are fixed as 13%, 6%, 3%, 5%, 0.1%, 2%, 2%, 1.3% respectively; The content of oil tea bacteriostatic extractive is as shown in table 1.

The content of table 1 containing compound P1 and P2 in the bath foam of oil tea bacteriostatic extractive

(2) according to extraordinary bath shampoo standard GB/T 19877.2 and Ministry of Public Health " disinfection technology standard ", adopt and detect fungistatic effect with the following method:

1. spawn culture

Escherichia coli are cultivated: the strain Escherichia coli of picking slant preservation is forwarded in the test tube that 10ml nutrient broth fluid medium is housed, 37 DEG C of quiescent culture 48-72h.

Staphylococcus aureus is cultivated: the staphylococcus aureus kind of picking slant preservation is forwarded in the test tube that 10ml nutrient broth fluid medium is housed, 37 DEG C of quiescent culture 18-24h.

2. bacteria suspension: depletion Staphylococcus aureus or escherichia coli 24h fresh cultured thing, with rinsing lower culture containing 1000mg/L peptone phosphate buffer, is mixed with required 1 × 10 ⁵the bacteria suspension of cfu/ml is for subsequent use.

3. test group: respectively the bath foam sample of the oil tea bacteriostatic extractive containing variable concentrations as shown in table 1 is made 50mm × 50mm size print, after 75% ethanol disinfection, be put in piecewise in sterile vessel, get 1.0ml test bacteria suspension drip contaminate in print central authorities, smoothen, make bacterium liquid and print edge leave the distance of 5mm, put 37 DEG C of incubator inner drying 30min, the antibacterial print as microbiological contamination is for subsequent use; Bacterium there is is to face up the antibacterial print of microbiological contamination smooth in sterile letheen planar surface; Use semi-solid agar 5.0ml, uniform fold, in microbiological contamination print surface, is put in 37 DEG C of incubators and is cultivated 24h, observed result, test repetition 3 times.

4. matched group: repeat above-mentioned steps 3., by step 3. in the bath foam sample of oil tea bacteriostatic extractive containing variable concentrations replace to existing formula bath gel (in the patent documentation being CN201310599343.X according to the patent No. embodiment 1 step prepared by bath gel), commercially available product Australia snow bath gel, test repetition 3 times.

5. blank group: test bacteria suspension is done suitably dilution, makes its concentration be 1 × 10 ³cfu/ml, gets its 0.1ml and drips to contaminate and smoothen on the homogeneity print not containing the bath foam of oil tea antibacterial substance, do after same process, with putting in a flat board, with semi-solid agar covering cultivation, as positive control with test group print; Simultaneously, test organisms suspension as count plate, and is observed not containing the cultivation counting of the tested bacterium of contrast print of oil tea antibacterial substance, test repetition 3 times in test.

The calculating of bacteriostasis rate: bacteriostasis rate=[(contrast average colony number-test average colony number)/contrast average colony number] × 100%.

(3) malicious combability measurements

Select the healthy mice 80 of body weight 20-25g, male and female half and half, be divided into 12 groups, comprise ten groups of test group, the bath foam giving clear water that accumulated dose is 20g/kg and the oil tea antibacterial substance containing variable concentrations for 2-3 time is divided in 24h, adopt administration by gavage, be inserted into white mouse gastric with syringe and inject, observe white mouse death condition.

(4) recruitment evaluation

Choose 400 volunteers, be divided into 12 groups, often organize 50 people, the bath oil of volunteer to the oil tea antibacterial substance containing variable concentrations is tried out, 30 days trial periods, use weekly the bath foam of the oil tea bacteriostatic extractive containing variable concentrations in (1), existing formula bath gel and commercially available product Australia snow bath gel 2-3 time respectively; Collect the evaluation of experimenter to pleasant sense project after de-sludging performance, skin pruritus suppression, bath, effective percentage=efficiently individual quantity/tested number × 100%.

Result of the test

(1) fungistatic effect test: the bacteriostatic test result of the bath foam of the oil tea bacteriostatic extractive containing variable concentrations is as shown in table 2, wherein, the bath foam of the oil tea bacteriostatic extractive of variable concentrations in the corresponding table 1 of 1-9 group difference.Result shows, bath foam containing bacteriostatic compound to the bacteriostasis rate of escherichia coli and staphylococcus aureus all more than 99%, wherein, the concentration of bacteriostatic compound is in the concentration range of 0.05-2%, and the fungistatic effect of the bath foam containing 0.1% compound P1 and 0.1% compound P1 is best.

The bacteriostatic test result of the different bath foam of table 2

(2) malicious combability measurements: the toxicity result of the test display of the bath foam of the oil tea bacteriostatic extractive containing variable concentrations: Continuous Observation seven days, none is dead for white mice, and has no abnormal symptom.Result of the test shows the median lethal dose(LD 50) LD of the bath foam of the bacteriostatic compound containing variable concentrations to male and female white mice ₅₀all be greater than 20g/kg, the nontoxic level in true border.

(3) recruitment evaluation: the recruitment evaluation of different bath foam is as shown in table 3, compared with avenging bath gel with existing formula bath gel and commercially available product Australia, the detergency of the bath foam containing bacteriostatic compound P1 and/or P2 is strong, foaming abundancy, antipruritic effect is obvious, after bathing, dermal sensation is pleasant, wherein, best with the combination property of the bath foam (the 4th group) containing 0.1% compound P1 and 0.1% compound P2.

The recruitment evaluation of the different bath foam of table 3

Embodiment 3

In order to further illustrate beneficial effect of the present invention, repeat the step (1) of embodiment 2, repeat the step (1) of embodiment 2, the withered powder of tea is also added in step (1), obtain bath foam A, the bath foam B and bath foam C that contain oil tea bacteriostatic extractive and the withered powder of tea, wherein, each component and percentage by weight as shown in table 4.

Each component and content thereof in table 4 bath foam

According to step (2)-(4) of embodiment 2, above-mentioned three kinds of bath foam are carried out fungistatic effect test, malicious combability measurements and recruitment evaluation.

Result of the test

(1) fungistatic effect test: the bacteriostatic test result of the bath foam of the oil tea antibacterial substance containing variable concentrations is as shown in table 5,

The bacteriostatic test result of the different bath foam of table 5

(2) malicious combability measurements: the toxicity result of the test display of the bath foam of the oil tea antibacterial substance containing variable concentrations: Continuous Observation seven days, none is dead for white mice, and has no abnormal symptom.Result of the test shows that the bath foam of the oil tea antibacterial substance containing variable concentrations is to the median lethal dose(LD 50) LD of male and female white mice ₅₀all be greater than 20g/kg, the nontoxic level in true border.

(3) recruitment evaluation: the recruitment evaluation result of different bath foam is as shown in table 6, three kinds of bath foam containing the withered powder of tea, oil tea bacteriostatic extractive all have that detergency is strong, antipruritic effect obviously, dermal sensation is pleasant after bathing feature; Wherein, best with the combination property of bath foam A (the withered powder of the tea containing 0.05%).

The recruitment evaluation of the different bath foam of table 6

The above; be only the present invention's preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.

Claims

1. the bath foam containing natural bacteriostatic active component, is characterized in that, by weight percentage, comprising:

PH adjusting agent is appropriate;

Surplus is water;

The chemical constitution of P2 is as shown in formula II:

2. the bath foam containing natural bacteriostatic active component as claimed in claim 1, is characterized in that, described chelating agen is at least one in disodiumedetate and tetrasodium ethylenediamine tetraacetate.

3. the bath foam containing natural bacteriostatic active component as claimed in claim 1 or 2, it is characterized in that, described skin protectant is at least one in ethylene glycol, glycerol and lanoline.

4. the bath foam containing natural bacteriostatic active component as claimed in claim 1, it is characterized in that, described thickening agent is at least one in ammonium chloride, hydroxyethyl-cellulose and sodium chloride.

5. the bath foam containing natural bacteriostatic active component as claimed in claim 1, is characterized in that, described containing in the bath foam of natural bacteriostatic active component, the percentage by weight of described bacteriostatic compound is 0.05-2% or 0.05%-1%.

6. the bath foam containing natural bacteriostatic active component as claimed in claim 1, is characterized in that, the described bath foam containing natural bacteriostatic active component also comprises frosting agent 0.01-1%.

7. frosting agent as claimed in claim 6, it is characterized in that, described frosting agent is the withered powder of tea.

8. a preparation method for the bath foam containing natural bacteriostatic active component, comprises the steps:

(1) polyoxyethylenated alcohol sodium sulfate, cocoanut fatty acid diethanolamide, cocamido propyl betaine, oil tea extract, skin protectant is soluble in water, mix homogeneously;

(2) step (1) gained mixture is heated to 60-80 DEG C, adds sodium lauryl sulphate, chelating agen, thickening agent, make it dissolve, and mix homogeneously, then, be cooled to room temperature;

(3) adopt pH adjusting agent that the pH value of step (2) gained mixture is adjusted to 5.0-6.0, obtain the bath foam containing oil tea antibacterial substance;

PH adjusting agent is appropriate;

Surplus is water;

The chemical constitution of P2 is as shown in formula II:

9. the preparation method of the bath foam containing natural bacteriostatic active component as claimed in claim 8, is characterized in that, described chelating agen is at least one in disodiumedetate and tetrasodium ethylenediamine tetraacetate.

10. the preparation method of the bath foam containing natural bacteriostatic active component as claimed in claim 8, is characterized in that, in described step (2), also comprise: