Preservative, preparation method thereof and cosmetic preservative

Abstract

The invention provides a preservative, a preparation method thereof and a cosmetic preservative, and belongs to the technical field of cosmetics. The invention discloses a tea polyphenol preservative which is prepared from the following raw materials in percentage by mass: 0.3-0.5% of tea polyphenol, 20-30% of an oil tea extract, 40-50% of a bamboo leaf extract, 5-10% of a pine needle extract and the balance of a solvent. According to the invention, the tea polyphenol, the camellia oleifera extract, the bamboo leaf extract and the pine needle extract are used as raw materials, and all the extracts have a synergistic effect, so that the preservative has remarkable antibacterial and preservative effects, small irritation and no toxic or side effect, and can be used as a cosmetic preservative.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and in particular to a preservative and a preparation method thereof and a cosmetic preservative. Background Art

[0002] The components of existing cosmetics include nutrients such as protein, vitamins, soluble collagen, oils and waxes. These nutrients provide favorable conditions for the reproduction of microorganisms. However, the large-scale reproduction of microorganisms will destroy the effective ingredients of cosmetics and cause the product to deteriorate. Therefore, preservatives play a vital role in the production process of cosmetics.

[0003] At present, although there are a large number of preservatives in the prior art, their antiseptic effects or safety are not satisfactory. For example, the preservatives commonly used in cosmetics on the market include parabens, methylisothiazolinone, methylchloroisothiazolinone and kason, etc., which are mostly chemical synthetic preservatives. Although such chemical preservatives have good antibacterial effects, they are highly irritating and easily cause skin allergies. Although some natural plant extract preservatives have certain safety, their antibacterial effects cannot reach the performance of chemical preservatives, which limits the application of natural plant extract preservatives.

[0004] Therefore, there is an urgent need to provide a preservative with low irritation, no toxic side effects and good antibacterial effect. Summary of the invention

[0005] The object of the present invention is to provide a preservative and a preparation method thereof and a cosmetic preservative. The preservative provided by the present invention has low irritation, no toxic side effects and good antibacterial effect, and can be used as a cosmetic preservative.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The invention provides a preservative, which is prepared from the following raw materials by mass content: 0.3-0.5% of tea polyphenols, 20-30% of camellia oleifera extract, 40-50% of bamboo leaf extract, 5-10% of pine needle extract and the remainder of solvent.

[0008] Preferably, the method for preparing the camellia oleifera extract comprises: sequentially performing withering, crushing and alcohol extraction on the camellia oleifera tissue, and then concentrating the obtained extract to a solid content of 60-80% to obtain the camellia oleifera extract.

[0009] Preferably, the solvent for the alcohol extraction is an ethanol solution, and the volume fraction of ethanol in the ethanol solution is 70-75%.

[0010] Preferably, the temperature of the alcohol extraction is 20-35° C., and the time of the alcohol extraction is 10-15 hours.

[0011] Preferably, the preparation method of the bamboo leaf extract comprises: extracting bamboo leaf powder with water and concentrating the extract to obtain the bamboo leaf extract.

[0012] Preferably, the water extraction temperature is 80-85° C., and the water extraction time is 1-3 hours.

[0013] Preferably, the method for preparing the pine needle extract comprises the following steps:

[0014] (1) extracting pine needle powder with ethanol to obtain an extract;

[0015] (2) dissolving the extract obtained in step (1) in water, and then extracting to obtain an extract;

[0016] (3) The extract obtained in step (2) is purified and dried in sequence to obtain a pine needle extract.

[0017] Preferably, the purification method in step (3) is a macroporous adsorption resin separation method.

[0018] The present invention also provides a method for preparing the preservative described in the above technical solution, comprising: mixing tea polyphenols, camellia oleifera extract, bamboo leaf extract, pine needle extract and a solvent to obtain a mixed solution; spray-drying the mixed solution to obtain the preservative.

[0019] The present invention also provides a cosmetic preservative, which is the preservative described in the above technical solution or the preservative prepared by the preparation method described in the above technical solution.

[0020] The present invention provides a preservative, which is prepared from the following raw materials by mass content: 0.3-0.5% tea polyphenols, 20-30% camellia extract, 40-50% bamboo leaf extract, 5-10% pine needle extract and the rest of solvent. The present invention uses tea polyphenols, camellia extract, bamboo leaf extract and pine needle extract as raw materials, and there is a synergistic effect between the extracts, and the antibacterial and antiseptic effects are significant, and the irritation is small, and there is no toxic side effect, and it can be used as a cosmetic preservative. The results of the embodiment show that the preservative provided by the present invention is non-irritating in multiple skin irritation tests on rabbits. The rabbits in the test group did not show irritation reactions such as erythema and edema on the test skin 24h and 48h after the stimulation of contact with the mixture, and the skin sensitization rate was 0%; the guinea pigs in the negative control group had no abnormalities in the test skin; and the antibacterial effect on a variety of bacteria was significant. DETAILED DESCRIPTION

[0021] The invention provides a preservative, which is prepared from the following raw materials by mass content: 0.3-0.5% of tea polyphenols, 20-30% of camellia oleifera extract, 40-50% of bamboo leaf extract, 5-10% of pine needle extract and the remainder of solvent.

[0022] In the present invention, the raw materials for preparing the preservative include tea polyphenols with a mass content of 0.3-0.5%, preferably 0.4-0.5%. In an embodiment of the present invention, the mass content of the tea polyphenols can be 0.3%, 0.4% or 0.5%. In the present invention, tea polyphenols contain a variety of phenolic substances, which not only have excellent antioxidant and antibacterial properties, but also can provide a synergistic effect on the antibacterial properties of other natural extracts, thereby improving the preservative effect of the preservative. The present invention does not specifically limit the source of the tea polyphenols, and conventional commercially available products can be used. In an embodiment of the present invention, the tea polyphenols come from Shaanxi Haochen Biotechnology Co., Ltd.

[0023] In the present invention, the raw material for preparing the preservative includes 20-30% by mass of camellia oleifera extract, preferably 25-30% by mass. In an embodiment of the present invention, the mass content of the camellia oleifera extract can be 20%, 25% or 30%. The present invention adds the camellia oleifera extract as a natural preservative component, which has little irritation and no toxic side effects.

[0024] In the present invention, the preparation method of the camellia oleifera extract comprises: sequentially performing withering, crushing and alcohol extraction on the camellia oleifera tissue, and then concentrating the obtained extract to a solid content of 60-80% to obtain the camellia oleifera extract.

[0025] In the present invention, the oil-tea camellia tissue preferably includes oil-tea camellia leaves and / or oil-tea camellia flowers. The use of oil-tea camellia leaves and / or oil-tea camellia flowers in the present invention is more conducive to obtaining oil-tea camellia extracts with high activity.

[0026] In the present invention, the method of killing green is preferably microwave. In an embodiment of the present invention, the power of the microwave can be 100W, and the time of the microwave can be 2 minutes. The present invention can passivate the oxidase activity in fresh plants by killing green, and inhibit the enzymatic oxidation of tea polyphenols in fresh leaves.

[0027] The present invention does not specifically limit the method of the pulverization, and a conventional pulverization method can be used. The present invention can improve the effect of alcohol extraction by pulverization. The present invention does not specifically limit the particle size after the pulverization, and it can be adjusted as needed. In an embodiment of the present invention, the pulverization is preferably passed through a 60-mesh sieve, and alcohol extraction is performed after obtaining the powder.

[0028] In the present invention, the solvent for the alcohol extraction is preferably an ethanol solution, and the volume fraction of ethanol in the ethanol solution is preferably 70-75%, more preferably 75%. The present invention uses an ethanol solution for alcohol extraction, which is more conducive to fully extracting the camellia oleifera extract from the camellia oleifera.

[0029] In the present invention, the alcohol extraction temperature is preferably 20-35°C, more preferably 25-30°C; the alcohol extraction time is preferably 10-15h, more preferably 12-15h. The present invention is more conducive to improving the effect of alcohol extraction at the above temperature and time.

[0030] The present invention does not specifically limit the amount of the solvent used in the alcohol extraction and the number of alcohol extractions, and can be adjusted as needed to fully extract the camellia oleifera extract. In an embodiment of the present invention, the number of alcohol extractions can be 2 times.

[0031] In the present invention, after the alcohol extraction, the obtained extract is preferably centrifuged, and the supernatant is concentrated. The present invention can separate the solid impurities from the liquid in the extract by centrifugation, thereby improving the purity of the extract. The present invention does not specifically limit the specific parameters of the centrifugation, as long as the solid impurities can be fully separated.

[0032] In the present invention, the concentration temperature is preferably 40-50°C, more preferably 40-45°C; the concentration method is preferably rotary evaporation. The present invention can remove the solvent of alcohol extraction by concentration to obtain the camellia oleifera extract.

[0033] In the present invention, the solid content of the concentrated extract is 60-80%, preferably 70-80%. The present invention controls the solid content after concentration within the above range, has less solvent residue, and has higher purity of the camellia oleifera extract.

[0034] In the present invention, the raw material for preparing the preservative includes 40-50% by mass of bamboo leaf extract, preferably 40-45%. In an embodiment of the present invention, the mass content of the bamboo leaf extract can be 40%, 45% or 50%. The present invention adds bamboo leaf extract as a natural preservative component, which has little irritation and no toxic side effects.

[0035] In the present invention, the preparation method of the bamboo leaf extract preferably comprises: extracting bamboo leaf powder with water, and concentrating the extract to obtain the bamboo leaf extract.

[0036] In the present invention, the ratio of the volume of water to the mass of bamboo leaf powder is preferably (20-25) mL: 1 g, and more preferably 25 mL: 1 g. In the present invention, the ratio of the volume of water to the mass of bamboo leaf powder is referred to as the solid-liquid ratio. The present invention controls the solid-liquid ratio within the above range, which is more conducive to fully extracting the bamboo leaf extract from the bamboo leaf powder.

[0037] The present invention has no special limitation on the particle size of the bamboo leaf powder, and conventional bamboo leaves can be crushed to obtain the powder. The present invention is more conducive to increasing the contact area with water and improving the water extraction effect by using bamboo leaf powder.

[0038] The present invention has no particular limitation on the water extraction method, and a conventional water extraction method may be used.

[0039] In the present invention, the water extraction temperature is preferably 80-85°C, more preferably 82-85°C; the water extraction time is preferably 1-3h, more preferably 2h. In an embodiment of the present invention, the water extraction can be performed twice. The present invention performs water extraction at the above temperature and time, which is more conducive to fully extracting the bamboo leaf extract from the bamboo leaf powder.

[0040] The present invention has no particular limitation on the temperature and time of the concentration, as long as water can be fully removed and the product obtained by water extraction forms a viscous extract.

[0041] In the present invention, the raw material for preparing the preservative includes pine needle extract with a mass content of 5-10%, preferably 8-10%. In an embodiment of the present invention, the mass content of the pine needle extract can be 5%, 8% or 10%. The present invention adds pine needle extract as a natural preservative component, which has little irritation and no toxic side effects.

[0042] In the present invention, the preparation method of the pine needle extract preferably comprises the following steps:

[0043] (1) extracting pine needle powder with ethanol to obtain an extract;

[0044] (2) dissolving the extract obtained in step (1) in water, and then extracting to obtain an extract;

[0045] (3) The extract obtained in step (2) is purified and dried in sequence to obtain a pine needle extract.

[0046] In the present invention, the pine needle powder is preferably subjected to ethanol extraction to obtain an extract.

[0047] In the present invention, the method for preparing the pine needle powder is preferably: drying and crushing the pine needles and then sieving to obtain the pine needle powder. In an embodiment of the present invention, the sieve opening of the sieving can be 60 meshes. The present invention is more conducive to increasing the contact area with ethanol and improving the extraction effect of the pine needle extract by preparing the pine needles into pine needle powder.

[0048] In the present invention, the volume fraction of ethanol is preferably 70-75%, more preferably 75%.

[0049] The present invention does not impose any special restrictions on the volume of the ethanol and the mass of the pine needle powder, and they can be selected according to a conventional extraction method.

[0050] In the present invention, the ethanol extraction is preferably carried out at room temperature, and the time of the ethanol extraction is preferably 18 to 24 hours, more preferably 20 to 24 hours.

[0051] The present invention preferably extracts the pine needle powder with ethanol for 18 to 24 hours, filters it, repeats the ethanol extraction for 3 times, combines the extracts, and concentrates the extracts to obtain an extract. The present invention does not specifically limit the volume of the concentrated extract, as long as the ethanol can be fully removed.

[0052] After obtaining the extract, the present invention preferably dissolves the extract in water and then extracts it to obtain an extract.

[0053] The present invention has no particular limitation on the amount of water used, as long as it can fully dissolve the extract.

[0054] In the present invention, the extraction reagent is preferably n-butanol. The present invention has no special limitation on the amount of n-butanol used, and it can be adjusted according to the extraction needs. The present invention preferably improves the extraction effect by multiple extractions. In an embodiment of the present invention, the number of extractions can be 3 times.

[0055] After obtaining the extract, the present invention preferably purifies and dries the extract in sequence to obtain the pine needle extract.

[0056] The present invention preferably concentrates the extract first and then purifies it. The present invention can reduce the volume of the solvent by concentration, making subsequent purification easier to operate. The present invention does not specifically limit the volume of the concentrated extract, and it can be adjusted as needed.

[0057] In the present invention, the purification method is preferably a macroporous adsorption resin separation method. In an embodiment of the present invention, the method of the macroporous adsorption resin separation method can be: loading the extract onto a macroporous resin adsorption column, washing impurities with water after adsorption saturation, and then eluting with an ethanol aqueous solution with a volume fraction of 80%, and collecting the eluate.

[0058] The present invention preferably concentrates the eluate and then vacuum dries it to obtain the pine needle extract. The present invention has no particular limitation on the concentration and drying method, as long as the solvent in the eluate can be fully removed to obtain the dry pine needle extract.

[0059] In the present invention, the raw materials for preparing the preservative include a solvent. In the present invention, the solvent is preferably propylene glycol. The present invention utilizes a solvent to evenly disperse the components.

[0060] The preservative provided by the present invention uses natural plant ingredients such as camellia oleifera extract and bamboo leaf extract as main raw materials, overcomes the allergen risk of traditional chemical preservatives, can reduce or delay the growth and reproduction of microorganisms, can be used as a preservative for cosmetics to delay the growth of microorganisms or corruption caused by chemical changes, inhibit the growth and reproduction of microorganisms, and extend the shelf life of cosmetics, with natural and safe effects; and, tea polyphenols, camellia oleifera extract, bamboo leaf extract and pine needle extract play a synergistic role, have a broad-spectrum antibacterial effect, good compatibility, and are non-toxic, non-irritating to the skin, have no skin allergic reaction, are easily degradable, and do not pollute the environment.

[0061] The present invention also provides a method for preparing the preservative described in the above technical solution, comprising: mixing tea polyphenols, camellia oleifera extract, bamboo leaf extract, pine needle extract and a solvent to obtain a mixed solution; spray-drying the mixed solution to obtain the preservative.

[0062] The present invention has no particular limitation on the method of mixing the tea polyphenols, camellia oleifera extract, bamboo leaf extract, pine needle extract and solvent, as long as the tea polyphenols, camellia oleifera extract, bamboo leaf extract and pine needle extract can be completely dissolved in the solvent.

[0063] The present invention has no special limitation on the amount of the solvent, which can be adjusted according to the amount of tea polyphenols, camellia oleifera extract, bamboo leaf extract and pine needle extract so that the tea polyphenols, camellia oleifera extract, bamboo leaf extract and pine needle extract can be completely dissolved in the solvent.

[0064] After obtaining the mixed solution, the present invention spray-dries the mixed solution to obtain the preservative.

[0065] The present invention has no special restrictions on the operation method and parameters of the spray drying. A conventional spray drying method can be used to form a dry powder from the mixed solution.

[0066] The method provided by the invention is simple and easy to operate, and can obtain a dry preservative.

[0067] The present invention also provides a cosmetic preservative, which is the preservative described in the above technical solution or the preservative prepared by the preparation method described in the above technical solution.

[0068] The preservative provided by the invention has the characteristics of low irritation, no toxic side effects and good antibacterial effect, so it can be used as a cosmetic preservative.

[0069] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0070] Example 1

[0071] A preservative is prepared from the following raw materials by weight: 0.4% tea polyphenols, 25% camellia extract, 45% bamboo leaf extract, 8% pine needle extract and propylene glycol (the sum of all components is 100%);

[0072] The preparation method of camellia oleifera extract is as follows: after picking camellia oleifera tea leaves and camellia oleifera flowers, they are sterilized by 100W microwave for 2 minutes, crushed to 60 mesh, extracted with 75% ethanol by volume, extracted at 30°C for 12 hours, and the extraction is repeated twice. After the extracts are combined, the supernatant is centrifuged and rotary evaporated at 45°C, and concentrated to a solid content of 70% to obtain the camellia oleifera extract.

[0073] Preparation method of bamboo leaf extract: add water to bamboo leaf powder with a solid-liquid ratio of 25mL:1g, perform water bath reflux extraction twice at 82°C, each extraction time is 2h, combine the two extracts, and concentrate them by reduced pressure distillation to a viscous state to obtain bamboo leaf extract.

[0074] Preparation method of pine needle extract:

[0075] (1) drying the pine needles, crushing them, passing them through a 60-mesh sieve, adding 75% ethanol by volume for extraction for 20 h, and then filtering; repeating this operation three times, combining the obtained filtrates, and concentrating them by rotary evaporation to obtain an extract;

[0076] (2) adding distilled water to dissolve the extract obtained in step (1), extracting with n-butanol, and releasing the n-butanol extract from the lower end of the separatory funnel; leaving the water layer in the funnel, continuing to add n-butanol for extraction, and repeating three times; combining the obtained n-butanol extracts, and concentrating under reduced pressure;

[0077] (3) The extract obtained in step (2) is loaded onto a macroporous resin adsorption column, and after adsorption saturation, impurities are washed away with water, and then eluted with an ethanol aqueous solution with a volume fraction of 80%, the eluate is collected, concentrated and vacuum dried to obtain a pine needle extract.

[0078] The preparation method of the preservative is as follows: accurately weigh the raw materials by mass percentage: 0.4% of tea polyphenols, 25% of camellia oleifera extract, 45% of bamboo leaf extract, 8% of pine needle extract, and the remainder is solvent propylene glycol (the sum of the mass percentages of each raw material is 100%); after mixing evenly, spray drying, and the obtained powder is the preservative.

[0079] Example 2

[0080] A preservative is prepared from the following raw materials by mass content: 0.5% tea polyphenols, 20% camellia extract, 40% bamboo leaf extract, 10% pine needle extract and propylene glycol (the sum of all components is 100%);

[0081] The preparation method of camellia oleifera extract is as follows: after picking camellia oleifera tea leaves and camellia oleifera flowers, they are sterilized by 100W microwave for 2 minutes, crushed to 60 mesh, extracted with 75% ethanol by volume, extracted at 20°C for 15 hours, and the extraction is repeated twice. After the extracts are combined, the supernatant is centrifuged and rotary evaporated at 40°C, concentrated to a solid content of 80%, and the camellia oleifera extract is obtained.

[0082] Preparation method of bamboo leaf extract: add water to bamboo leaf powder with a solid-liquid ratio of 25mL:1g, perform water bath reflux extraction twice at 80°C, each extraction time is 2h, combine the two extracts, and concentrate them by reduced pressure distillation to a viscous state to obtain bamboo leaf extract.

[0083] Preparation method of pine needle extract:

[0084] (1) drying the pine needles, crushing them, passing them through a 60-mesh sieve, adding ethanol to extract for 18 hours, and then filtering; repeating this operation three times, combining the obtained filtrates, and concentrating them by rotary evaporation to obtain an extract;

[0085] (2) adding distilled water to dissolve the extract obtained in step (1), extracting with n-butanol, and releasing the n-butanol extract from the lower end of the separatory funnel; leaving the water layer in the funnel, continuing to add n-butanol for extraction, and repeating three times; combining the obtained n-butanol extracts, and concentrating under reduced pressure;

[0086] (3) The extract obtained in step (2) is loaded onto a macroporous resin adsorption column, and after adsorption saturation, impurities are washed away with water, and then eluted with an ethanol aqueous solution with a volume fraction of 80%, the eluate is collected, concentrated and vacuum dried to obtain a pine needle extract.

[0087] The preparation method of the preservative is as follows: accurately weigh the raw materials by mass percentage: 0.5% of tea polyphenols, 20% of camellia oleifera extract, 40% of bamboo leaf extract, 10% of pine needle extract, and the remainder is solvent propylene glycol (the sum of the mass percentages of each raw material is 100%); after uniform mixing, spray drying is performed, and the obtained powder is the preservative.

[0088] Example 3

[0089] A preservative is prepared from the following raw materials by weight: 0.3% tea polyphenols, 30% camellia extract, 40% bamboo leaf extract, 5% pine needle extract and propylene glycol (the sum of all components is 100%);

[0090] The preparation method of camellia oleifera extract is as follows: after picking camellia oleifera tea leaves and camellia oleifera flowers, they are sterilized by 100W microwave for 2 minutes, crushed to 60 mesh, extracted with 75% ethanol by volume, extracted at 35°C for 10 hours, and the extraction is repeated twice. After the extracts are combined, the supernatant is centrifuged and rotary evaporated at 50°C, and concentrated to a solid content of 60% to obtain the camellia oleifera extract.

[0091] Preparation method of bamboo leaf extract: add water to bamboo leaf powder with a solid-liquid ratio of 25mL:1g, perform water bath reflux extraction twice at 85°C, each extraction time is 2h, combine the two extracts, and concentrate them by reduced pressure distillation to a viscous state to obtain bamboo leaf extract.

[0092] Preparation method of pine needle extract:

[0093] (1) drying the pine needles, crushing them and passing them through a 60-mesh sieve, adding ethanol to extract for 24 hours, and then filtering; repeating this operation three times, combining the obtained filtrates, and concentrating them by rotary evaporation to obtain an extract;

[0094] (2) adding distilled water to dissolve the extract obtained in step (1), extracting with n-butanol, and releasing the n-butanol extract from the lower end of the separatory funnel; leaving the water layer in the funnel, continuing to add n-butanol for extraction, and repeating three times; combining the obtained n-butanol extracts, and concentrating under reduced pressure;

[0095] (3) The extract obtained in step (2) is loaded onto a macroporous resin adsorption column, and after adsorption saturation, impurities are washed away with water, and then eluted with an ethanol aqueous solution with a volume fraction of 80%, the eluate is collected, concentrated and vacuum dried to obtain a pine needle extract.

[0096] The preparation method of the preservative is as follows: accurately weigh the raw materials by mass percentage: 0.3% of tea polyphenols, 30% of camellia oleifera extract, 40% of bamboo leaf extract, 5% of pine needle extract, and the remainder is solvent propylene glycol (the sum of the mass percentages of each raw material is 100%); after mixing evenly, spray drying, and the obtained powder is the preservative.

[0097] Test Case

[0098] The preservative prepared in Example 1 was subjected to acute oral toxicity test, skin irritation test and skin allergy test, and the test method was as follows:

[0099] (1) Acute oral toxicity test: healthy rats (180g-220g) were selected for the test for 14 days. The weight difference between individual experimental animals of the same sex should not exceed 20% of the average weight. The rats should adapt to the test environment for at least 3 days before the test. 4-5 dose groups were set up, each with 10 animals, half male and half female. It was found that the dose of 5000 mg / kg did not cause animal death.

[0100] (2) Skin irritation test and multiple skin irritation test: select rabbits with no less than 4 rabbits per group; use the left and right side self-comparison method, apply the preservative directly to the prepared skin, and cover and fix it with a dressing; the application time is at least 4 hours; in the multiple-dose skin irritation test, the application is continued on the same part, with the same application time each time, for a period of 14 days; in the damaged skin test, the degree of skin damage is limited to damage to the epidermis; observe the skin reaction with the naked eye under full-spectrum light; the observation time points for the single-dose skin irritation test are 50 minutes, 24 hours, 48 ​​hours and 72 hours after the removal of the preservative; the multiple-dose skin The irritation test was conducted 1 hour after each removal of preservatives, before each application of preservatives, and 50 minutes, 24 hours, 48 ​​hours and 72 hours after the last application of preservatives. As negative control animals, 20 white guinea pigs were selected, half of which were male and half were female, with a body weight of 280±10g, 10 in each group, and they were first adapted to breeding in the laboratory for 1 week. The positive allergen was 2,4-dinitrochlorobenzene, and the sensitizing and stimulating concentrations were 10 mg / mL and 8 mg / mL, respectively. The results of the acute oral toxicity test are shown in Table 1, the results of the skin irritation test are shown in Table 2, and the results of the multiple skin irritation tests are shown in Table 3.

[0101] Table 1 Results of acute oral toxicity test

[0102]

[0103] Table 2 Skin irritation test results

[0104]

[0105]

[0106] As can be seen from Table 2, the results of the multiple skin irritation tests on rabbits prepared by the present invention are non-irritating. No irritation reactions such as erythema and edema were observed on the test skin of the rabbits in the test group 24h and 48h after the stimulation of contact with the mixture, and the skin sensitization rate was 0%; no abnormalities were observed on the test skin of guinea pigs in the negative control group.

[0107] Table 3 Results of multiple skin irritation tests

[0108]

[0109] In Table 3, the positive substance used in the positive control group* was 2,4-dinitrochlorobenzene (the sensitizing and stimulating concentrations were 10 mg / mL and 8 mg / mL, respectively).

[0110] As can be seen from Table 3, the results of the guinea pig skin allergy test of the preservative prepared by the present invention showed that no skin allergy was observed, indicating that the preservative prepared by the present invention has little irritation to the skin and has no toxic side effects.

[0111] Test Example 2

[0112] Evaluation method and results of antibacterial activity of preservatives: The antibacterial zone was determined by agar plate punching method. Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Bacillus subtilis and Candida albicans were used as test strains, and the above test strains were diluted with sterile saline to a bacterial suspension with a concentration of 106CFU / mL. Prepare beef extract peptone medium, malt extract medium and potato glucose agar medium, sterilize at 121℃ for 20min, cool to 50±2℃, pour into a plate (plate diameter is 90mm), shake well, and condense; take 150μL of the above bacterial suspension and add it to the corresponding culture medium, then spread it evenly with a coating rod and set aside. Under sterile conditions, a sterile hole puncher with a diameter of 6 mm was used to punch holes on the prepared bacterial plate, and then the agar block was picked out with sterilized tweezers, and then 40 μL of the preservative prepared in Example 1 of the present invention, plant extract (tea camellia extract, bamboo leaf extract and pine needle extract, all of which are taken as examples of the products prepared in Example 1) and solvent were added to each hole, and cultured in a constant temperature incubator. After the culture was completed, the antibacterial effect was observed and the diameter of the antibacterial zone (mm) was measured. Three parallel experiments were performed, and the average value was taken. The results are shown in Table 4.

[0113] Table 4 Antibacterial test results of preservatives

[0114] Staphylococcus aureus Bacillus subtilis Pseudomonas aeruginosa Escherichia coli Candida albicans Example 1 20.60±0.10 14.01±0.02 14.11±0.21 11.20±0.11 10.56±0.13 Camellia oleifera extract 14.12±0.31 9.12±0.19 10.34±0.24 10.22±0.19 6.27±0.58 Bamboo Leaf Extract 13.40±0.40 9.24±0.08 6.00±0.00 9.30±0.41 6.00±0.00 Pine Needle Extract 11.70±0.06 9.43±0.11 10.12±0.80 6.00±0.00 7.51±0.10 Propylene glycol 6.00±0.00 6.00±0.00 6.00±0.00 6.00±0.00 6.00±0.00

[0115] In Table 4, Example 1 refers to the preservative prepared in Example 1.

[0116] It can be seen from Table 4 that the antibacterial effect of the preservative prepared by the present invention is significantly better than that of a single plant extract, and has significant effects on multiple bacteria. This indicates that there is a synergistic effect between the extracts of the preservative provided by the present invention, which improves the antibacterial effect of the preservative.

[0117] Test Example 3

[0118] The antiseptic effect of the preservative prepared by the present invention in cream cosmetics:

[0119] (1) Experimental group setting

[0120] The experiment was divided into 4 groups, the components are as follows:

[0121] The first group: no preservative was added; the second group: 1.25 wt% of the preservative prepared in Example 1 was added; the third group: 2.5 wt% of the preservative prepared in Example 1 was added; the fourth group: 0.5 wt% of phenoxyethanol was added.

[0122] The formula of the cream cosmetics used in this test example is shown in Table 5.

[0123] Table 5 Formula of cream cosmetics

[0124]

[0125]

[0126] (2) Experimental methods

[0127] Take 10g of a preservative-free cream with a basic formula (see Table 5), add the preservative prepared in Example 1 of the present invention to the sample so that the final preservative content in the sample is 1.25wt% and 2.5wt%, respectively, and then mix thoroughly for use. Set the cream without preservative as a blank sample and add 0.5wt% phenoxyethanol as a preservative control sample. Store the prepared samples at room temperature for 28 days, and take samples at regular intervals to determine the total number of colonies according to the experimental method recommended by the Cosmetic and Flavor Association (CTFA).

[0128] The experimental results of comparing the preservative effects of cosmetics with and without preservatives are shown in Table 6.

[0129] Table 6 Experimental results of the antiseptic effect of cosmetics with and without preservatives

[0130]

[0131] As shown in Table 6, after adding the cosmetic preservative phenoxyethanol, the products were not contaminated with bacteria under the experimental conditions of 28 days; the first group of products without adding the preservative were contaminated with bacteria on the 21st day; the second and third groups to which the preservative prepared by the present invention was added were not contaminated with bacteria under the experimental conditions of 28 days, indicating that the preservative prepared by the present invention has a preservative effect on cosmetics.

[0132] It can be seen from the above results that the preservative provided by the present invention has low irritation, no toxic side effects and good antibacterial effect, so it can be used as a cosmetic preservative to solve the problems of high irritation of chemical synthetic preservatives and poor antibacterial effect of natural plant extract preservatives.

[0133] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A preservative, which is prepared from the following raw materials by mass content: 0.3-0.5% tea polyphenols, 20-30% camellia extract, 40-50% bamboo leaf extract, 5-10% pine needle extract and the remainder solvent.

2. The preservative according to claim 1, characterized in that The preparation method of the camellia oleifera extract comprises: sequentially performing withering, crushing and alcohol extraction on camellia oleifera tissue, and then concentrating the obtained extract to a solid content of 60-80% to obtain the camellia oleifera extract.

3. The preservative according to claim 2, characterized in that The solvent for the alcohol extraction is an ethanol solution, and the volume fraction of ethanol in the ethanol solution is 70-75%.

4. The preservative according to claim 2 or 3, characterized in that The temperature of the alcohol extraction is 20-35° C., and the time of the alcohol extraction is 10-15 hours.

5. The preservative according to claim 1, characterized in that The preparation method of the bamboo leaf extract comprises: extracting bamboo leaf powder with water and concentrating the bamboo leaf extract.

6. The preservative according to claim 5, characterized in that The water extraction temperature is 80-85° C., and the water extraction time is 1-3 hours.

7. The preservative according to claim 1, characterized in that The preparation method of the pine needle extract comprises the following steps: (1) extracting pine needle powder with ethanol to obtain an extract; (2) dissolving the extract obtained in step (1) in water, and then extracting to obtain an extract; (3) The extract obtained in step (2) is purified and dried in sequence to obtain a pine needle extract.

8. The preservative according to claim 7, characterized in that The purification method in step (3) is a macroporous adsorption resin separation method.

9. A method for preparing the preservative according to any one of claims 1 to 8, comprising: Mixing tea polyphenols, camellia oleifera extract, bamboo leaf extract, pine needle extract and a solvent to obtain a mixed solution; The mixed solution is spray-dried to obtain a preservative.

10. A cosmetic preservative, which is the preservative according to any one of claims 1 to 8 or the preservative prepared by the preparation method according to claim 9.

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