Preservative for cosmetics and preparation process thereof

Abstract

The invention relates to the technical field of cosmetic additives, in particular to a preservative for cosmetics. The preservative is prepared from the following components in parts by weight: 2 to 4 parts of lotus leaf extract, 3 to 6 parts of wild chrysanthemum flower extract, 2 to 4 parts of green tea extract, 2 to 3 parts of blueberry extract, 3 to 5 parts of orange peel extract, 13 to 20 parts of lingnanine extract, 13 to 20 parts of arunine extract, 10 to 15 parts of chitosan compound, 1 to 3 parts of stabilizer, 1 to 3 parts of thickener, 1 to 2 parts of antioxidant and 1 to 3 parts of tea tree essential oil. The preservative comprises 1-3 parts of chamomile extract, 1-3 parts of black tea essence and 60-70 parts of water, and further relates to a process for preparing the preservative through the formula, and growth and reproduction of more types of bacteria and fungi can be effectively inhibited.

Description

Technical Field

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

[0002] Cosmetics are fine chemical products used to clean, protect, beautify or change the appearance of the human body. They have complex ingredients and are prone to the growth of microorganisms. Therefore, preservatives need to be added to inhibit the growth of bacteria, molds and yeasts, extend the shelf life and ensure safety. Common preservatives include traditional chemical preservatives (such as parabens, phenoxyethanol, etc.) and natural preservatives (such as plant extracts and biological fermentation products). Although preservatives play an important role in ensuring the safety of cosmetics, some chemical preservatives may cause skin allergies and other problems. Therefore, in recent years, consumers' demand for natural preservatives and products without added preservatives has gradually increased.

[0003] The invention patent with application number 201310461594.1 discloses a compound preservative for cosmetics, which is made of the following raw materials in parts by weight: 1-5 parts of lavender, 1-4 parts of calendula, 1-3 parts of scutellaria, 1-3 parts of peony root, 3-5 parts of rosemary, 1-3 parts of cloves, and 3-5 parts of licorice; its preparation method is to crush the raw materials in the formula and mix them, add ethanol, extract 1-3 times under water bath conditions, each extraction is 1-3 hours, combine the extracts, filter, decompress the filtrate to recover ethanol, and dry to obtain. The present invention selects pure natural plants and Chinese herbal medicines with preservative effects, and compound them into preservatives, which can effectively inhibit the growth of microorganisms such as bacteria and fungi in cosmetics, extend the service life of cosmetics, are safe and non-toxic to the human body, and also have the advantages of anti-oxidation, whitening and anti-inflammatory.

[0004] However, the above technology can only inhibit a limited number of fungi. If a variety of cosmetics need to be used for preservation, or the users are in different regions, the same product may be contaminated by different fungi under different usage environments. Therefore, a technology is needed that can effectively inhibit the growth and reproduction of more types of bacteria and fungi. Summary of the invention

[0005] The present invention provides a cosmetic preservative and a preparation process thereof, which can effectively inhibit the growth and reproduction of more types of bacteria and fungi.

[0006] In order to solve the above technical problems, the present application provides the following technical solutions: a preservative for cosmetics and a preparation process thereof, which comprises, by mass percentage, 2-4 parts of lotus leaf extract, 3-6 parts of wild chrysanthemum extract, 2-4 parts of green tea extract, 2-3 parts of blueberry extract, 3-5 parts of orange peel extract, 13-20 parts of amaryllis nicotinic acid extract, 13-20 parts of lycopodiella citrate extract, 10-15 parts of chitosan complex, 1-3 parts of stabilizer, 1-3 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of tea tree essential oil, 1-3 parts of chamomile extract, 1-3 parts of black tea essence, and 60-70 parts of water.

[0007] The basic principle and beneficial effects of this scheme: This scheme uses the synergistic antibacterial effect of multiple plant extracts: lotus leaf extract contains alkaloids such as nuciferine, which has anti-mitotic effects and can interfere with the cell division process of microorganisms to inhibit their growth; wild chrysanthemum extract is rich in flavonoids, which can destroy the cell membrane structure and function of microorganisms and affect their material transport and metabolism. The two synergistically enhance the inhibitory ability against bacteria and fungi. Tea polyphenols in green tea extract and flavonoids in orange peel extract also inhibit the growth and reproduction of microorganisms through similar mechanisms, such as binding to the enzyme system of microorganisms and changing the pH value of the intracellular environment, forming a multi-target antibacterial defense line.

[0008] Synergistic effect of natural alkaloids and complexes: Amaryllis alkaloid extract and arundinaceous alkaloid extract have antibacterial activity, and they interact with chitosan complexes. Chitosan complexes can be adsorbed on the surface of microorganisms and change the permeability of microbial cells, while alkaloids further interfere with the internal physiological processes of microorganisms, such as inhibiting protein synthesis and destroying genetic material. This synergistic effect significantly enhances the overall antibacterial effect of preservatives, enabling them to effectively deal with various types of microbial contamination.

[0009] Stabilizing effect of antioxidant ingredients: Anthocyanins in blueberry extract, tea polyphenols in green tea extract, and antioxidants (such as vitamin C, vitamin E, etc.) can capture free radicals in cosmetics and prevent oxidation reactions caused by free radicals. Oxidation reactions can cause problems such as rancidity of fats and decomposition of active ingredients in cosmetics. Antioxidant ingredients block oxidation chain reactions, maintain the chemical stability of cosmetics, extend the shelf life of the product, and maintain the activity of its effective ingredients.

[0010] This solution is highly safe: it is composed of natural plant extracts and bioactive ingredients, which greatly reduces the risk of skin irritation and allergies compared to traditional chemical synthetic preservatives. For example, when cosmetics containing this preservative are used for a long time, it is not easy to cause adverse reactions such as skin redness, itching, and inflammation. It is suitable for people with sensitive skin and provides consumers with safer cosmetic options. Rich skin care effects: in addition to the antiseptic function, it also has skin care effects such as antioxidant, antibacterial and anti-inflammatory, and soothing. In the daily use of cosmetics, it can not only prevent product deterioration, but also help improve skin condition, such as reducing skin inflammation, resisting free radical damage to the skin, and promoting the healthy metabolism of skin cells, etc., to achieve the dual role of skin care and antiseptic, and improve the overall quality of cosmetics. Environmentally friendly and sustainable: the raw materials are mainly derived from plants, and the pollution to the environment during production and use is relatively small, which is in line with the concept of environmental protection and sustainable development. Unlike some chemical preservatives that are difficult to degrade, these natural ingredients are easier to decompose in the natural environment, reducing the potential harm to the ecosystem, and are conducive to promoting the green development of the cosmetics industry. Wide range of applications: Through reasonable formula design, it can adapt to the formulation requirements of different types of cosmetics, such as lotions, creams, essences, toners, etc. Whether it is a water-based or oily system, it can effectively play a preservative role and will not affect the texture, color and smell of cosmetics, providing a universal preservative solution for cosmetics manufacturers, reducing R&D and production costs.

[0011] Furthermore, the stabilizer is one of glycerol, propylene glycol, sorbitol, sodium benzoate or vitamin E.

[0012] Furthermore, the thickener is one of xanthan gum, gelatin, carrageenan or oat glucan.

[0013] Furthermore, the antioxidant is one of vitamin C, vitamin E, β-carotene, tea polyphenols, quercetin or rosemary extract.

[0014] A process for preparing a preservative for cosmetics comprises the following steps:

[0015] S1: Raw material preparation: wash and dry lotus leaves, wild chrysanthemum, green tea, blueberry and orange peel, grind them separately, pass through a 40-mesh sieve to obtain powder of each plant material, and set aside;

[0016] S2: Extracting hydrosol: Select rosemary stems, leaves and flowers or mint leaves as plant materials; put the plant materials into a distiller, add an appropriate amount of water, and then heat to boiling. The generated water vapor carries the aroma molecules of the plant materials and condenses into liquid to obtain hydrosol;

[0017] S3: Extracting various plant extracts: obtaining extracts of lotus leaf, wild chrysanthemum, green tea, blueberry, and orange peel, and preparing them separately;

[0018] S4: extracting amaryllis nicotinic acid;

[0019] S5: extracting gramine;

[0020] S6: preparing chitosan composite;

[0021] S7: Prepare preservatives: by mass percentage, take 2-4 parts of lotus leaf extract, 3-6 parts of wild chrysanthemum extract, 2-4 parts of green tea extract, 2-3 parts of blueberry extract, 3-5 parts of orange peel extract, 13-20 parts of amaryllis alkaloid extract, 13-20 parts of argyrine extract, 10-15 parts of chitosan complex, 1-3 parts of stabilizer, 1-3 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of tea tree essential oil, 1-3 parts of chamomile extract, 1-3 parts of black tea essence, mix with hydrosol, the hydrosol is 60-70 parts;

[0022] S8: Quality testing: by testing the preservatives for appearance, pH value, stability, and microorganisms;

[0023] S9: Packing and storage.

[0024] Further, the extraction method of each plant extract in step S3 is:

[0025] Lotus leaf extract: add lotus leaf powder to 8-10 times of its weight of water, decoct 1-3 times, decoct for 1-3 hours each time, combine the decoctions, filter and concentrate to a crude drug concentration of 1-1.3g / ml;

[0026] Wild chrysanthemum extract: add wild chrysanthemum powder to water 8-10 times its weight, decoct 1-3 times, decoct for 1-3 hours each time, combine the decoctions, filter and concentrate to a crude drug concentration of 1-1.3g / ml;

[0027] Green tea extract: green tea powder is added to an ethanol solution of 8-10 times its weight, soaked for 24-48 hours, filtered and concentrated, and then purified by chromatography;

[0028] Blueberry extract: blueberries are dried and crushed, soaked in an acidic aqueous solution 6-8 times their weight for 12-24 hours, filtered and concentrated to obtain;

[0029] Orange peel extract: Wash the orange peel, dry it and crush it, add 5-7 times of its weight of organic solvent, extract it by ultrasonic for 30-60 minutes, filter and concentrate it.

[0030] Further, the extraction step of amaryllis nicotinic acid in step S4 is:

[0031] S41: Raw material collection: Collect the bulbs of Amaryllis;

[0032] S42: Pretreatment: washing, cutting or grinding the amaryllis bulbs;

[0033] S43: Extraction: Extraction is performed using a suitable solvent at room temperature or after heating;

[0034] S44: Concentration: The extract is concentrated by evaporation or reverse osmosis;

[0035] S45: Purification: The purification process includes chromatography, crystallization, recrystallization, extraction, and washing;

[0036] S46: Identification and quantification: The extracts were identified and quantified by chemical analysis methods.

[0037] Further, the extraction step of gramine in step S5 is:

[0038] S51: Raw material preparation: First, you need to prepare the roots, stems and leaves of Phragmites australis;

[0039] S52: Pretreatment: washing, cutting or grinding the roots, stems and leaves of Phragmites australis;

[0040] S53: Extraction: Extraction of plant material using water or alcohol, with the extraction process repeated multiple times;

[0041] S54: Separation and purification: The extract is filtered and centrifuged to remove impurities, and can then be further purified by chromatography, crystallization, recrystallization, etc.;

[0042] S55: Identification and quantification: The extracts were identified and quantified by chemical analysis methods.

[0043] Further, the preparation steps of the chitosan complex in step S6 are:

[0044] S61: Pretreatment: Cleaning, crushing and grinding of crustacean shells;

[0045] S62: Acid-base treatment: Acid-base treatment is used to remove impurities in chitosan and improve its purity, and this step is repeated multiple times;

[0046] S63: activated carbon pretreatment: washing, drying and crushing the activated carbon to obtain processed activated carbon;

[0047] S63: Combining: putting chitosan into an acetic acid aqueous solution to swell, adding the treated activated carbon, dispersing evenly, adding acetaldehyde or epichlorohydrin as a cross-linking agent, mixing evenly, cross-linking reacting at 50-100° C. for 0.5-3 hours, and then washing and drying to obtain a finished activated carbon / chitosan composite;

[0048] S64: Drying: further drying the prepared chitosan composite product;

[0049] S65: Screening and packaging: Screening and packaging of chitosan complex. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] Figure 1 It is a cross-sectional view of Example 1 of a cosmetic preservative and its preparation process; DETAILED DESCRIPTION

[0051] The following is further described in detail through specific implementation methods:

[0052] A formula of a cosmetic preservative comprises, by mass percentage, 2-4 parts of lotus leaf extract, 3-6 parts of wild chrysanthemum extract, 2-4 parts of green tea extract, 2-3 parts of blueberry extract, 3-5 parts of orange peel extract, 13-20 parts of amaryllis nicotinic acid extract, 13-20 parts of gramineous alkaloid extract, 10-15 parts of chitosan complex, 1-3 parts of stabilizer, 1-3 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of tea tree essential oil, 1-3 parts of chamomile extract, 1-3 parts of black tea essence and 60-70 parts of water.

[0053] As attached Figure 1 As shown, a process for preparing a cosmetic preservative comprises the following steps:

[0054] S1: Raw material preparation: wash and dry lotus leaves, wild chrysanthemum, green tea, blueberry and orange peel, grind them separately, pass through a 40-mesh sieve to obtain powder of each plant material, and set aside;

[0055] S2: Extracting hydrosol: Select rosemary stems, leaves and flowers or mint leaves as plant materials; put the plant materials into a distiller, add an appropriate amount of water, and then heat to boiling. The generated water vapor carries the aroma molecules of the plant materials and condenses into liquid to obtain hydrosol;

[0056] S3: Extracting various plant extracts: obtaining extracts of lotus leaf, wild chrysanthemum, green tea, blueberry, and orange peel, and preparing them separately;

[0057] Lotus leaf extract: add lotus leaf powder to 8-10 times of its weight of water, decoct 1-3 times, decoct for 1-3 hours each time, combine the decoctions, filter and concentrate to a crude drug concentration of 1-1.3g / ml;

[0058] Wild chrysanthemum extract: add wild chrysanthemum powder to water 8-10 times its weight, decoct 1-3 times, decoct for 1-3 hours each time, combine the decoctions, filter and concentrate to a crude drug concentration of 1-1.3g / ml;

[0059] Green tea extract: green tea powder is added to an ethanol solution of 8-10 times its weight, soaked for 24-48 hours, filtered and concentrated, and then purified by chromatography;

[0060] Blueberry extract: blueberries are dried and crushed, soaked in an acidic aqueous solution 6-8 times their weight for 12-24 hours, filtered and concentrated to obtain;

[0061] Orange peel extract: Wash the orange peel, dry it and crush it, add 5-7 times of its weight of organic solvent, extract it by ultrasonic for 30-60 minutes, filter and concentrate it.

[0062] S4: extracting amaryllis nicotinic acid;

[0063] S41: Raw material collection: Collect the bulbs of Amaryllis;

[0064] S42: Pretreatment: washing, cutting or grinding the amaryllis bulbs;

[0065] S43: Extraction: Extraction is performed using a suitable solvent at room temperature or after heating;

[0066] S44: Concentration: The extract is concentrated by evaporation or reverse osmosis;

[0067] S45: Purification: The purification process includes chromatography, crystallization, recrystallization, extraction, and washing;

[0068] S46: Identification and quantification: The extracts were identified and quantified by chemical analysis methods.

[0069] S5: extracting gramine;

[0070] S51: Raw material preparation: First, you need to prepare the roots, stems and leaves of Phragmites australis;

[0071] S52: Pretreatment: washing, cutting or grinding the roots, stems and leaves of Phragmites australis;

[0072] S53: Extraction: Extraction of plant material using water or alcohol, with the extraction process repeated multiple times;

[0073] S54: Separation and purification: The extract is filtered and centrifuged to remove impurities, and can then be further purified by chromatography, crystallization, recrystallization, etc.;

[0074] S55: Identification and quantification: The extracts were identified and quantified by chemical analysis methods.

[0075] S6: preparing chitosan composite;

[0076] S61: Pretreatment: Cleaning, crushing and grinding of crustacean shells;

[0077] S62: Acid-base treatment: Acid-base treatment is used to remove impurities in chitosan and improve its purity, and this step is repeated multiple times;

[0078] S63: activated carbon pretreatment: washing, drying and crushing the activated carbon to obtain processed activated carbon;

[0079] S63: Combining: putting chitosan into an acetic acid aqueous solution to swell, adding the treated activated carbon, dispersing evenly, adding acetaldehyde or epichlorohydrin as a cross-linking agent, mixing evenly, cross-linking reacting at 50-100° C. for 0.5-3 hours, and then washing and drying to obtain a finished activated carbon / chitosan composite;

[0080] S64: Drying: further drying the prepared chitosan composite product;

[0081] S65: Sieving and packaging: Sieving and packaging of chitosan complexes

[0082] S7: Prepare preservatives: by mass percentage, take 2-4 parts of lotus leaf extract, 3-6 parts of wild chrysanthemum extract, 2-4 parts of green tea extract, 2-3 parts of blueberry extract, 3-5 parts of orange peel extract, 13-20 parts of amaryllis alkaloid extract, 13-20 parts of rutin extract, 10-15 parts of chitosan complex, 1-3 parts of stabilizer, 1-3 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of tea tree essential oil, 1-3 parts of chamomile extract, 1-3 parts of black tea essence, and mix with hydrosol, the hydrosol is 60-70 parts; the antioxidant is one of vitamin C, vitamin E, β-carotene, tea polyphenols, quercetin or rosemary extract. The stabilizer is one of glycerin, propylene glycol, sorbitol, sodium benzoate or vitamin E. The thickener is one of xanthan gum, gelatin, carrageenan or oat glucan.

[0083] First, prepare a strictly cleaned and disinfected mixing container to ensure that there are no impurities and microbial residues inside the container to prevent the quality of the preservative from being affected. According to the mass percentage, use a high-precision electronic scale to weigh 2-4 parts of lotus leaf extract, 3-6 parts of wild chrysanthemum extract, 2-4 parts of green tea extract, 2-3 parts of blueberry extract, 3-5 parts of orange peel extract, 13-20 parts of amaryllis alkaloid extract, 13-20 parts of rutin extract, 10-15 parts of chitosan complex, 1-3 parts of stabilizer, 1-3 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of tea tree essential oil, 1-3 parts of chamomile extract, and 1-3 parts of black tea essence, and place the weighed solid and liquid components in clean containers for use. First, slowly add the solid components to the mixing container, gently stir during the addition process, so that the solid components are evenly distributed at the bottom of the container to avoid caking. Next, pour the liquid ingredients dropwise or slowly into the container, turn on the low-speed stirring device at the same time, set the stirring speed to 100-200 rpm to prevent the liquid from splashing and producing too much foam. Measure 60-70 parts of hydrosol and slowly add it to the above-mentioned mixed system. The addition speed of the hydrosol should be moderate, and continuous stirring should be carried out during the addition process to ensure that the hydrosol is fully mixed with other ingredients. Increase the stirring speed to 300-500 rpm, and the stirring time is 20-40 minutes to further mix the ingredients under high-speed stirring. Ultrasonic treatment is performed on the mixture, and the ultrasonic frequency is set to 20-40kHz for 10-20 minutes. The cavitation generated during the ultrasonic process can promote the dispersion and dissolution of the ingredients, so that the interaction between the ingredients is more sufficient. Adjust the stirring speed to 100-300 rpm again, and continue stirring for 30-60 minutes to make the texture of the preservative more delicate and uniform, and ensure that a stable system is formed between the ingredients.

[0084] After the mixing is completed, the prepared preservatives are sampled and tested to check whether the pH value is within the appropriate range of 4.5-6.5 and whether the content of each component meets the predetermined ratio. If the pH value is not within the specified range, an appropriate amount of acid-base regulator can be used to adjust it; if the content of the component is deviated, the corresponding component should be supplemented or reduced according to the corresponding calculation results until all indicators meet the requirements.

[0085] S8: Quality testing: by testing the preservatives for appearance, pH value, stability, and microorganisms;

[0086] S9: Packing and storage.

[0087] Example

[0088] Embodiment 1:

[0089] Formula ratio: Lotus leaf extract: 2 parts, wild chrysanthemum extract: 3 parts, green tea extract: 2 parts, blueberry extract: 2 parts, orange peel extract: 3 parts, amaryllis alkaloid extract: 13 parts, lycopodiella citrate extract: 13 parts, chitosan complex: 10 parts, stabilizer (glycerin): 1 part, thickener (xanthan gum): 1 part, antioxidant (vitamin C): 1 part, tea tree essential oil: 1 part, chamomile extract: 1 part, black tea essence: 1 part, water: 60 parts

[0090] Preparation process and results:

[0091] Prepared according to standard process. First, prepare the raw materials, wash and dry the lotus leaf, wild chrysanthemum, green tea, blueberry and orange peel, and crush them through a 40-mesh sieve respectively. When extracting each plant extract, the lotus leaf extract is prepared by adding lotus leaf powder to 8 times its weight of water, decocting 3 times, decocting for 2 hours each time, filtering after combining the decoction, and concentrating the filtrate under reduced pressure to a crude drug concentration of 1g / ml. The obtained extract is darker in color and dark green and viscous. Wild chrysanthemum extract is also added with 8 times of water, decocted 3 times, 2 hours each time, and filtered and concentrated to have a strong medicinal fragrance. Green tea extract adds green tea powder to 8 times of ethanol solution, soaks for 36 hours, concentrates after filtration, and then obtains it through purification steps such as chromatography separation, and finally obtains a light green clear liquid. Blueberry extract pulverizes blueberries after drying, soaks them in an acidic aqueous solution (pH 4) 6 times their weight for 18 hours, and concentrates after filtration to obtain a purple-red semi-solid. Orange peel extract: Wash the orange peel, dry it and crush it, add ethyl acetate 5 times its weight, ultrasonically extract for 40 minutes, filter and concentrate to obtain a fresh fruity aroma.

[0092] The preparation of amaryllis alkaloid extract is to collect the bulbs of Amaryllis, wash and cut them, and then extract them with methanol at room temperature. The extract is evaporated, concentrated, chromatographically purified, crystallized, and finally obtains a high-purity extract. The roots, stems, and leaves of Phragmites australis are prepared for the preparation of alkaloid extract. After washing and grinding, they are extracted with alcohol multiple times and obtained by filtering, centrifugation, chromatographic purification, and other operations. The preparation of chitosan complex is to first wash, crush and grind the shells of crustaceans, remove impurities through multiple acid and alkali treatments, and then add acetaldehyde cross-linking agent to the treated activated carbon and swollen chitosan, cross-linking reaction at 70°C for 2 hours, and then wash, dry, sieve and package to obtain the finished product.

[0093] When preparing the preservative, first slowly add the solid component to the disinfected preparation container and gently stir evenly, then add the liquid component dropwise, and turn on the low-speed stirring device of 150 rpm at the same time. Then measure 60 parts of pure dew and slowly add it, continue stirring, then increase the stirring speed to 400 rpm and stir for 30 minutes, then perform ultrasonic treatment (frequency 30kHz, time 15 minutes), and finally stir at 200 rpm for 45 minutes. The prepared preservative is a light yellow uniform liquid with a pH value of 5.2. According to microbial detection, the diameter of the antibacterial circle for Escherichia coli is 17mm, the diameter of the antibacterial circle for Staphylococcus aureus is 15mm, and the diameter of the antibacterial circle for Candida albicans is 14mm, which has a good antibacterial effect. After storage at 40°C for 3 months, there is no obvious change in the appearance of the preservative, and the content of the effective ingredient is maintained at more than 95% by high performance liquid chromatography analysis.

[0094] Embodiment 2:

[0095] Recipe ratio:

[0096] Lotus leaf extract: 2.5 parts, wild chrysanthemum extract: 4 parts, green tea extract: 2.5 parts, blueberry extract: 2.2 parts, orange peel extract: 3.5 parts, amaryllis alkaloid extract: 15 parts, rutinine extract: 15 parts, chitosan complex: 11 parts, stabilizer (propylene glycol): 1.5 parts, thickener (gelatin): 1.5 parts, antioxidant (vitamin E): 1.2 parts, tea tree essential oil: 1.5 parts, chamomile extract: 1.5 parts, black tea essence: 1.5 parts, water: 63 parts

[0097] Preparation process and results:

[0098] The raw material preparation steps are the same as those in Example 1. When extracting lotus leaf extract, add lotus leaf powder to water 9 times its weight, decoct 3 times, decoct for 2.5 hours each time, and concentrate to a crude drug concentration of 1.1 g / ml. The amount of extract obtained is larger and the color is slightly lighter than that in Example 1. The amount of water used in wild chrysanthemum extract is increased to 9 times the raw material, and the number of decoctions is still 3 times, each time for 2 hours. After filtering and concentration, the fragrance is strong. When the green tea extract is soaked in ethanol, the ethanol concentration is increased by 5%, and the soaking time is shortened to 30 hours. The color of the extract obtained after purification is lighter. When the blueberry extract is crushed, a more sophisticated equipment is used to make its particle size smaller. It is soaked in an acidic aqueous solution (pH 4.2) 7 times its weight for 16 hours, filtered and concentrated, and the viscosity of the obtained extract is slightly lower. When the orange peel extract is ultrasonically extracted, the time is extended to 50 minutes, and the fragrance of the extract is stronger.

[0099] The preparation process of amaryllis alkaloid extract and arundinaceous alkaloid extract was fine-tuned in the amount of extraction solvent and extraction time to improve the extraction efficiency and purity. In the preparation process of chitosan composite, the number of washing times was increased during the pretreatment of activated carbon to ensure the purity of the activated carbon, and the cross-linking reaction was carried out at 80°C for 1.5 hours.

[0100] When deploying preservative, strictly follow the steps, add solid first and then liquid, the low-speed stirring speed is 180 rev / min, and the hydrosol is first stirred at high speed for 35 minutes (450 rev / min) after adding, the ultrasonic treatment frequency is 35kHz, the time is 12 minutes, and finally the low-speed stirring is 50 minutes (250 rev / min). The color of the preservative after deployment is slightly darker than Example 1, which is a yellow transparent liquid, and the pH value is 5.4. The diameter of the antibacterial circle for Escherichia coli reaches 19mm, the diameter of the antibacterial circle for Staphylococcus aureus is 17mm, and the diameter of the antibacterial circle for Candida albicans is 16mm. After storage at 45°C for 3 months, the appearance is stable, and the remaining 96% of the active ingredient content is detected, and after mixing with toner, the clarity and stability of toner can be maintained, and no turbidity, precipitation or peculiar smell occurs during the shelf life.

[0101] Embodiment 3:

[0102] Formula ratio: Lotus leaf extract: 3 parts, wild chrysanthemum extract: 4.5 parts, green tea extract: 3 parts, blueberry extract: 2.5 parts, orange peel extract: 4 parts, amaryllis alkaloid extract: 17 parts, lycopodiella citrate extract: 17 parts, chitosan complex: 13 parts, stabilizer (sodium benzoate): 2 parts, thickener (carrageenan): 2 parts, antioxidant (β-carotene): 1.5 parts, tea tree essential oil: 2 parts, chamomile extract: 2 parts, black tea essence: 2 parts, water: 66 parts

[0103] Preparation process and results:

[0104] After the raw materials are prepared, the amount of water used in the lotus leaf extract is increased to 10 times its weight during extraction, the number of decoctions is reduced to 2 times, each decoction lasts for 3 hours, and the vacuum degree and temperature are adjusted during concentration to reach a crude drug concentration of 1.2g / ml. The texture of the obtained extract is relatively uniform. The wild chrysanthemum extract adopts a continuous extraction process to improve the extraction efficiency and the purity of the extract. The green tea extract optimizes the ratio and flow rate of the eluent in the chromatographic separation and purification step, and the obtained extract has a higher content of active ingredients. The temperature and humidity of the blueberry extract are strictly controlled during the drying and crushing process to ensure the quality and stability of the extract. The orange peel extract is subjected to secondary extraction after organic solvent extraction, using the same organic solvent but increasing the extraction time and ultrasonic power, which further improves the extraction rate of the active ingredient.

[0105] New solvent combinations were tried in the extraction process of amaryllis alkaloid extract to improve the extraction selectivity and purity. The number of crystallizations in the separation and purification steps of arundinaceous alkali extract was increased to make the product purer. The preparation of chitosan complexes precisely controlled the acid-base concentration and treatment time during acid-base treatment, controlled the crushing particle size during activated carbon pretreatment, and carried out the cross-linking reaction at 90°C for 1 hour to ensure product quality.

[0106] When the preservative is prepared, each step is operated in a standardized manner, the low-speed stirring speed is 160 rpm, the high-speed stirring is 40 minutes (500 rpm) after the hydrosol is added, the ultrasonic treatment frequency is 25kHz, the time is 18 minutes, and the final low-speed stirring is 40 minutes (220 rpm). The prepared preservative is a light yellow translucent liquid with a pH value of 5.3. The diameter of the antibacterial zone for Escherichia coli is 20 mm, the diameter of the antibacterial zone for Staphylococcus aureus is 18 mm, and the diameter of the antibacterial zone for Candida albicans is 17 mm. After being stored at 50°C for 3 months, the preservative has no precipitation and stratification phenomenon, and the content of the effective ingredient is still above 95% through detection. When used in a facial cream, it does not affect the texture, color and smearing feeling of the facial cream, and the facial cream maintains good stability and appearance during the shelf life.

[0107] Embodiment 4:

[0108] Formula ratio: lotus leaf extract: 3.5 parts, wild chrysanthemum extract: 5 parts, green tea extract: 3.5 parts, blueberry extract: 2.8 parts, orange peel extract: 4.5 parts, amaryllis alkaloid extract: 18 parts, lycopodiella citrate extract: 18 parts, chitosan complex: 14 parts, stabilizer (vitamin E): 2.5 parts, thickener (oat glucan): 2.5 parts, antioxidant (quercetin): 1.8 parts, tea tree essential oil: 2.5 parts, chamomile extract: 2.5 parts, black tea essence: 2.5 parts, water: 68 parts

[0109] Preparation process and results:

[0110] The lotus leaf extract adopts dynamic countercurrent extraction technology during extraction, which improves the extraction efficiency and the content of effective ingredients. The vacuum concentration method is adopted during concentration, and the crude drug concentration is quickly reached at a lower temperature. 1.25g / ml, the extract is bright in color. The number of decoctions of wild chrysanthemum extract is increased to 4 times, each decoction is 1.5 hours, the amount of water is 8.5 times that of the raw material, and the extraction effect is good. The green tea extract adopts a circulating soaking system during the ethanol soaking process to make the effective ingredients more fully dissolved, and the subsequent purification steps are also optimized. The obtained extract has high purity and pure color. When the blueberry extract is soaked in an acidic aqueous solution, the soaking temperature and stirring speed are adjusted to make the extraction process more efficient. The extract obtained after filtration and concentration is of excellent quality. The ultrasonic power and frequency of the orange peel extract are increased during ultrasonic extraction, and the selection and dosage of organic solvents are optimized at the same time, and the content of the effective ingredients in the extract is significantly improved.

[0111] The new separation technology was introduced in the purification process of Amaryllis alkaloid extract, which improved the purity and yield of the product. The plant material was pretreated in the extraction process of Achyranthes alkali extract, which enhanced the extraction effect and the purification steps were more stringent. The preparation of chitosan complex was finely controlled in each link, such as the temperature and time of acid-base treatment, the nature and dosage of activated carbon, and the conditions of cross-linking reaction, to ensure the stability of product quality.

[0112] When preparing the preservative, strictly follow the process, the low-speed stirring speed is 170 rpm, the high-speed stirring is 38 minutes (480 rpm) after the hydrosol is added, the ultrasonic treatment frequency is 32kHz, the time is 16 minutes, and finally the low-speed stirring is 48 minutes (230 rpm). The preservative obtained is a yellow transparent liquid with a pH value of 5.6. The diameter of the antibacterial zone for Escherichia coli reaches 21mm, the diameter of the antibacterial zone for Staphylococcus aureus is 19mm, and the diameter of the antibacterial zone for Candida albicans is 18mm. After storage at 55°C for 3 months, the appearance and active ingredient content remain stable. When used in emulsion, it can enhance the moisturizing performance and stability of the emulsion. The emulsion did not show stratification, deterioration and other phenomena during storage, and the smearing feeling was also improved.

[0113] Embodiment 5:

[0114] Formula ratio: lotus leaf extract: 4 parts, wild chrysanthemum extract: 6 parts, green tea extract: 4 parts, blueberry extract: 3 parts, orange peel extract: 5 parts, amaryllis alkaloid extract: 20 parts, lycopodiella citrate extract: 20 parts, chitosan complex: 15 parts, stabilizer (sorbitol): 3 parts, thickener (xanthan gum): 3 parts, antioxidant (rosemary extract): 2 parts, tea tree essential oil: 3 parts, chamomile extract: 3 parts, black tea essence: 3 parts, water: 70 parts

[0115] Preparation process and results:

[0116] After the raw materials were processed, the water quality of the lotus leaf extract was controlled during the extraction process, deionized water was used and the heating rate of the decoction was adjusted, so that the extract obtained had a high content of active ingredients and good stability. The wild chrysanthemum extract used supercritical fluid extraction technology, which greatly improved the extraction efficiency and the purity of the extract. A small amount of auxiliary solvent was added to the green tea extract during ethanol soaking to enhance the extraction effect, and the subsequent purification steps such as chromatographic separation were also optimized. The blueberry extract used vacuum freeze-drying technology during the drying process to avoid the loss of active ingredients, control the particle size within a narrower range during crushing, and optimize the soaking process parameters during soaking in acidic aqueous solution, so that the quality of the extract obtained was excellent. The orange peel extract was combined with microwave-assisted technology during ultrasonic extraction to improve the extraction rate, and was subjected to multiple refining treatments after organic solvent extraction.

[0117] The extraction and purification process of Amaryllis alkaloid extract uses automated equipment and advanced analytical testing methods to ensure the consistency and stability of product quality. The process parameters of the arundinaceous extract are optimized throughout the preparation process to improve the purity and yield of the product. The preparation of chitosan complexes strictly follows high standards in all links, such as the pretreatment of crustacean shells, precise control of acid and alkali treatment, high-quality preparation of activated carbon, and optimized conditions for cross-linking reactions, resulting in excellent product performance.

[0118] When preparing the preservative, follow the standard operation, the low-speed stirring speed is 190 rpm, the high-speed stirring is 36 minutes (460 rpm) after the hydrosol is added, the ultrasonic treatment frequency is 38kHz, the time is 14 minutes, and the final low-speed stirring is 52 minutes (240 rpm). The prepared preservative is a dark yellow translucent liquid with a pH value of 5.8. The diameter of the antibacterial zone for Escherichia coli is 23mm, the diameter of the antibacterial zone for Staphylococcus aureus is 21mm, and the diameter of the antibacterial zone for Candida albicans is 20mm. After storage at 60°C for 3 months, the stability of the preservative is good. The content of the active ingredient is maintained at more than 94% through testing. When used in the essence, it can effectively extend the shelf life of the essence without affecting its efficacy. The essence remains clear and transparent during storage, and the active ingredient is stable.

[0119] In this scheme, lotus leaf extract: contains alkaloids such as nuciferine, has anti-mitotic effect, can effectively inhibit the growth and reproduction of microorganisms, and provides basic antibacterial ability for preservatives. Wild chrysanthemum extract: rich in flavonoids, can destroy the cell membrane structure and function of microorganisms, enhance the inhibitory effect of preservatives on bacteria and fungi, and expand the antibacterial spectrum. Green tea extract: its tea polyphenol components have antioxidant and antibacterial properties, which can not only prevent the oxidation and deterioration of the ingredients in cosmetics, but also inhibit the growth of microorganisms and extend the shelf life of cosmetics. Blueberry extract: contains ingredients such as anthocyanins, has antioxidant and certain antibacterial effects, and helps to maintain the stability of cosmetics and skin care effects. Orange peel extract: flavonoids and other ingredients have antioxidant, antibacterial and anti-inflammatory properties, further enhancing the function of preservatives. Amaryllis nitramine extract and rutin extract: have antibacterial activity themselves, and work synergistically with other ingredients to enhance the inhibitory ability against microorganisms. Chitosan complex: can be adsorbed on the surface of microorganisms, change the permeability of microbial cells, and enhance the overall antiseptic effect. Stabilizer: Maintains the stability of the product, prevents the ingredients from deteriorating, separating or fading, ensures the effectiveness and safety of the cosmetics, and extends the shelf life. Thickener: Increases the viscosity and stability of the product, improves the texture and spreadability of the product, and enhances moisturizing and ductility. Antioxidant: Protects cosmetics from free radical damage, synergizes with other antioxidant ingredients, and enhances the antioxidant properties of preservatives. Tea tree essential oil: Has natural antibacterial ability, can effectively inhibit the growth of microorganisms, and adds antibacterial effects to preservatives. Chamomile extract: Has antibacterial and anti-inflammatory ingredients, can reduce inflammation, make the skin smoother and more comfortable, and can provide moisture retention for the skin. Black tea essence: The tea polyphenols contained have a strong antioxidant effect, which can help extend the shelf life of cosmetics and prevent the growth of microorganisms.

[0120] The water in Examples 1-5 is all hydrosol.

[0121] Taking the technology of patent application No. 201310461594.1 as a comparative example, the experimental results of Example 3 thereof are selected, namely:

[0122] Comparative Example: Preparation of a composite preservative for cosmetics: 3 kg of lavender, 2.5 kg of calendula, 2 kg of scutellaria, 2 kg of peony root, 4 kg of rosemary, 2.5 kg of cloves and 4 kg of licorice are crushed and mixed in a container, 70% ethanol by volume is added, and the amount added is 11 times the total weight of the raw materials. Extract twice in a water bath at 70°C, each extraction for 2.5 hours, combine the extracts, filter, reduce the pressure on the filtrate to recover the ethanol, and dry to obtain the product.

[0123] The antibacterial activity of the preservative of the present invention was determined by the paper disc method, and the specific test process is as follows:

[0124] 1. Test methods

[0125] Escherichia coli and Staphylococcus aureus were inoculated into broth culture medium and cultured at 37°C for 24 hours; Candida albicans was inoculated into Shabao weak liquid medium and cultured at 25°C for 5 days; Aspergillus niger was inoculated into Czapek liquid medium and cultured at 25°C for 6 days. Staphylococcus epidermidis: Pick a single colony and inoculate it into nutrient agar (TSA) or TSB liquid medium, and culture it at 37°C for 24 hours; when expanding the culture, inoculate it into TSB medium at a volume ratio of 1%, and culture it at 37°C and 220rpm for 12 hours. Pseudomonas aeruginosa: Pick a single colony from the plate and inoculate it into ordinary agar medium or MacConkey agar, and culture it at 37°C for 18-24 hours. The colony is flat and moist, and may be bright green due to pigment secretion; after culturing on blood agar for 24 hours, a hemolytic ring may appear around it. Penicillium expansum: slant culture medium (glucose 5g / L, peptone 5g / L, yeast powder 5g / L, agar 20g / L) was cultured at 28℃ for 48 hours for activation; seed culture medium (glucose 5g / L, peptone 5g / L, yeast powder 5g / L) was cultured at 28℃ for 30 hours; fermentation culture medium (glucose 10g / L, peptone 10g / L, yeast powder 10g / L, sodium chloride 3g / L) was cultured at 28℃, 180rpm shaker for 40 hours. Seven bacterial cultures were diluted with physiological saline to a bacterial suspension with a concentration of 106CFU / ml. The above four bacterial suspensions were spread on nutrient agar plates with sterile cotton swabs to make bacterial lawns, and then sterilized filter paper discs with a diameter of 3cm were taken, and the preservatives made in the comparative example and Example 5 were evenly dipped, and then attached to the plates made of four different bacterial suspensions. Bacteria were cultured for 24h, fungi were cultured for 5d, and the results were observed.

[0126] 2. Evaluation method:

[0127] The antibacterial diameter of the paper strip method is ≥10mm and is effective, while the antibacterial diameter is <10mm and is ineffective.

[0128] 3. Test results are shown in Table 1

[0129]

[0130] Table 1 Antibacterial effect of paper disc method preservatives

[0131] From the above results, it can be seen that this scheme not only has a good inhibitory effect on Escherichia coli, Staphylococcus aureus, Candida albicans, and Aspergillus niger, but also has a good inhibitory effect on Staphylococcus epidermidis, Pseudomonas aeruginosa, Penicillium expansum, etc.

[0132] The above are only embodiments of the present invention. The invention is not limited to the fields involved in this implementation case. The common sense such as the known specific structures and characteristics in the scheme is not described in detail here. The ordinary technicians in the relevant field know all the common technical knowledge in the technical field to which the invention belongs before the application date or the priority date, can obtain all the existing technologies in the field, and have the ability to apply the conventional experimental means before that date. The ordinary technicians in the relevant field can improve and implement this scheme in combination with their own abilities under the enlightenment given by this application. Some typical known structures or known methods should not become obstacles for ordinary technicians in the relevant field to implement this application. It should be pointed out that for those skilled in the art, without departing from the structure of the present invention, several deformations and improvements can be made, which should also be regarded as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicality of the patent. The protection scope required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to explain the content of the claims.

Claims

1. A cosmetic preservative and its preparation process, characterized in that: In terms of mass percentage, the lotus leaf extract is 2 - 4 parts, the wild chrysanthemum extract is 3 - 6 parts, the green tea extract is 2 - 4 parts, the blueberry extract is 2 - 3 parts, the orange peel extract is 3 - 5 parts, the amaryllis alkaloid extract is 13 - 20 parts, the gramineous alkaloid extract is 13 - 20 parts, the chitosan complex is 10 - 15 parts, the stabilizer is 1 - 3 parts, the thickener is 1 - 3 parts, the antioxidant is 1 - 2 parts, the tea tree essential oil is 1 - 3 parts, the chamomile extract is 1 - 3 parts, the black tea essence is 1 - 3 parts, and the water is 60 - 70 parts.

2. A cosmetic preservative according to claim 1, characterized in that: The stabilizer is one of glycerol, propylene glycol, sorbitol, sodium benzoate or vitamin E.

3. A cosmetic preservative according to claim 1, characterized in that: The thickener is one of xanthan gum, gelatin, carrageenan or oat glucan.

4. A cosmetic preservative according to claim 1, characterized in that: The antioxidant is one of vitamin C, vitamin E, beta-carotene, tea polyphenols, quercetin or rosemary extract.

5. A process for preparing a preservative for cosmetics: characterized in that: The following steps are involved: S1: Raw material preparation: Wash and dry lotus leaves, wild chrysanthemums, green tea, blueberries, and orange peels, grind them separately, and pass them through a 40-mesh sieve to obtain powders of each plant material for later use; S2: Extracting hydrosol: Select rosemary stems, leaves and flowers or mint leaves as plant materials; put the plant materials into a distiller, add an appropriate amount of water, and then heat to boiling. The generated water vapor carries the aroma molecules of the plant materials and condenses into liquid to obtain hydrosol; S3: Extracting various plant extracts: obtaining extracts of lotus leaf, wild chrysanthemum, green tea, blueberry, and orange peel, and preparing them separately; S4: extracting amaryllis nicotinic acid; S5: extracting gramine; S6: preparing chitosan composite; S7: preparing preservatives: by mass percentage, take 2-4 parts of lotus leaf extract, 3-6 parts of wild chrysanthemum extract, 2-4 parts of green tea extract, 2-3 parts of blueberry extract, 3-5 parts of orange peel extract, 13-20 parts of amaryllis alkaloid extract, 13-20 parts of rutinine extract, 10-15 parts of chitosan complex, 1-3 parts of stabilizer, 1-3 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of tea tree essential oil, 1-3 parts of chamomile extract, 1-3 parts of black tea essence, mix with hydrosol, the hydrosol is 60-70 parts; S8: Quality testing: by testing the preservatives for appearance, pH value, stability, and microbiology; S9: Packing and storage.

6. A process for preparing a cosmetic preservative according to claim 5, characterized in that: The extraction method of each plant extract in step S3 is: Lotus leaf extract: add lotus leaf powder to 8-10 times of its weight of water, decoct 1-3 times, 1-3 hours each time, combine the decoctions, filter and concentrate to a crude drug concentration of 1-1.3g / ml; Wild chrysanthemum extract: add wild chrysanthemum powder to 8-10 times of its weight of water, decoct 1-3 times, decoct for 1-3 hours each time, combine the decoctions, filter and concentrate to a crude drug concentration of 1-1.3g / ml; Green tea extract: Add green tea powder to an ethanol solution of 8 to 10 times its weight, soak for 24 to 48 hours, filter and concentrate, and then obtain through a purification step of chromatography separation; Blueberry extract: Dried blueberries are crushed, soaked in an acidic aqueous solution 6 to 8 times their weight for 12 to 24 hours, filtered and concentrated to obtain; Orange peel extract: Wash the orange peel, dry it and crush it, add 5-7 times its weight of organic solvent, extract it by ultrasonic for 30-60 minutes, filter and concentrate it.

7. The process for preparing a cosmetic preservative according to claim 5, characterized in that: The extraction steps of amaryllis alkaloids in step S4 are as follows: S41: Raw material collection: Collect the bulbs of Amaryllis; S42： Pretreatment: Wash, cut or grind the amaryllis bulbs; S43: Extraction: Extraction is performed using a suitable solvent, and the extraction process is performed at room temperature or after heating; S44: Concentration: The extract is concentrated by evaporation or reverse osmosis; S45： Purification: The purification process includes chromatography, crystallization, recrystallization, extraction, and washing; S46: Identification and quantification: The extracts were identified and quantified by chemical analysis methods.

8. The process for preparing a cosmetic preservative according to claim 5, characterized in that: The extraction steps of gramine in step S5 are: S51: Raw material preparation: First, you need to prepare the roots, stems and leaves of Phragmites australis; S52: Pretreatment: washing, cutting or grinding the roots, stems and leaves of Phragmites australis; S53: Extraction: Extraction of plant material using water or alcohol, with the extraction process repeated multiple times; S54: Separation and purification: The extract is filtered and centrifuged to remove impurities, and can then be further purified by chromatography, crystallization, recrystallization, etc.; S55: Identification and quantification: Identification and quantification of the extracts were performed by chemical analysis methods.

9. The process for preparing a cosmetic preservative according to claim 5, characterized in that: The preparation steps of the chitosan complex in step S6 are: S61: Pretreatment: Cleaning, crushing and grinding of crustacean shells; S62: Acid-base treatment: Acid-base treatment is used to remove impurities in chitosan and improve its purity, and this step is repeated multiple times; S63: activated carbon pretreatment: washing, drying and crushing the activated carbon to obtain processed activated carbon; S63: Combining: putting chitosan into an acetic acid aqueous solution to swell, adding the treated activated carbon, dispersing evenly, then adding acetaldehyde or epichlorohydrin as a cross-linking agent, mixing evenly, cross-linking reacting at 50-100° C. for 0.5-3 hours, then washing and drying to obtain a finished activated carbon / chitosan composite; S64: Drying: further drying the prepared chitosan composite product; S65: Screening and packaging: Screening and packaging of chitosan complex.

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