Preparation method of sunscreen microspheres with biological activity as well as product and application of sunscreen microspheres

Abstract

The invention relates to a preparation method of sunscreen microspheres with biological activity and a product and application of the sunscreen microspheres with the biological activity. The preparation method comprises the steps that titanium dioxide and zinc oxide are mixed, and a first mixture is obtained; inoculating a yeast strain into a fermentation culture medium, and mixing the yeast strain with the first mixture and a fermentation suspending agent for fermentation to obtain a turbid liquid; and carrying out spray drying on the suspension to obtain the product. And the titanium dioxide-zinc oxide mixture can uniformly wrap the yeast fermentation product, so that through biological fermentation, the environment-friendly property is good, the coating and the absorption are easy, and the skin is mild and non-irritating.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics and relates to a preparation method of sunscreen microspheres with biological activity and a product and application thereof. Background Art

[0002] With the popularization of cosmetic knowledge, people's understanding of the harm of ultraviolet rays continues to deepen, and daily sun protection has gradually received attention from consumers. Traditional physical sunscreens are mainly titanium dioxide and zinc oxide, which mainly protect the skin by reflecting and scattering ultraviolet radiation. Their main ingredients are usually some minerals. Chemical sunscreens are mainly oxybenzones, avobenzones, hexyltriazines, diisopropyl phthalate, octylbenzone and benzophenones, which mainly protect the skin by absorbing the energy of ultraviolet radiation and converting it into harmless heat or light energy.

[0003] Many sunscreen products use a combination of physical and chemical sunscreens in their formula design, taking advantage of the complementary absorption bands of different sunscreens to achieve a high SPF and broad-spectrum protection. However, various physical and chemical sunscreens often have safety risks, insufficient photostability, and poor feel. For example, some chemical sunscreens (such as AVB) are easily absorbed through the skin, which raises safety concerns and has poor photostability; while physical sunscreens (such as titanium dioxide) are nano-sized particles, which pose a risk of accumulation in hair follicles, and are prone to whitening and poor skin feel.

[0004] Modern sunscreen technology not only focuses on providing sunscreen effects, but also pays attention to the product's user experience, non-irritation and long-term stability, as well as its impact on the environment. Therefore, the research and development of sunscreen products continues to innovate on the basis of the above technologies to meet the needs and expectations of different groups of people for sunscreen protection. Summary of the invention

[0005] In view of the deficiencies of the prior art, the object of the present invention is to provide a method for preparing sunscreen microspheres with biological activity, and its products and applications.

[0006] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0007] In a first aspect, the present invention provides a method for preparing sunscreen microspheres having biological activity, the preparation method comprising:

[0008] (1) mixing titanium dioxide and zinc oxide to obtain a first mixture;

[0009] (2) inoculating the yeast strain into a fermentation medium, mixing and fermenting the mixture with the first mixture and a fermentation suspension to obtain a suspension;

[0010] (3) Spray-dry the suspension to obtain the product.

[0011] The present invention designs a sunscreen microsphere with a mixed powder of titanium dioxide and zinc oxide adsorbed on the surface and a biological whitening agent yeast fermentation product wrapped inside, so as to solve the safety and single effect of physical sunscreen. The microsphere can wrap and stabilize the active ingredients of the sunscreen to prevent them from decomposing or failing in the product, thereby prolonging the protective effect of the product. The microsphere can slowly release the sunscreen ingredients to form a lasting protective film on the skin surface, prolonging the sunscreen effect time of the product. The use of microspheres can improve the skin feel and smoothness of the product, make the product easier to be evenly applied on the skin, and reduce the oil film feeling. Traditional physical sunscreens usually leave a visible white film on the skin due to their relatively large particle size, especially when used in high concentrations. The microspheres can reduce or cover the white residue of the sunscreen itself, making the sunscreen product more transparent and natural on the skin. The dispersion and release mechanism of the microspheres in the product can ensure that the active ingredients are evenly distributed on the skin, avoiding uneven sunscreen effects in local areas. In general, sunscreen microspheres are not only for improving the appearance and feel of the product, but more importantly, they use technical means to improve the stability and protective effect of sunscreen products, so that they can more effectively protect the skin from UV damage.

[0012] Preferably, the mass ratio of titanium dioxide to zinc oxide is (5-10):(2-5).

[0013] The specific point values ​​in (5-10) can be selected as 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, etc., and the specific point values ​​in (2-5) can be selected as 2, 2.5, 3, 3.5, 4, 4.5, 5, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be listed here one by one.

[0014] Preferably, the yeast inoculation amount is 5-10%, and the viable bacteria count is 1×10 9 CFU / mL-1×10 10 CFU / mL.

[0015] The inoculation amount can be selected from 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, etc., and the viable cell count can be selected from 1×10 9 CFU / mL, 2×10 9 CFU / mL, 3×10 9 CFU / mL, 4×10 9 CFU / mL, 5×10 9 CFU / mL, 6×10 9 CFU / mL, 7×10 9 CFU / mL, 8×10 9 CFU / mL, 9×10 9CFU / mL, 1×10 10 CFU / mL, etc. Other specific point values ​​within the above numerical range can be selected and will not be described here one by one.

[0016] Preferably, the yeast comprises Saccharomyces cerevisiae.

[0017] Preferably, the volume ratio of the fermentation medium, the first mixture and the fermentation suspension is (10-20):(1-2):(1-2).

[0018] Among them, the specific point values ​​in (10-20) can be selected as 10, 10.5, 11, 11.5, 12, 12.5, 13, 13.5, 14, 14.5, 15, 15.5, 16, 16.5, 17, 17.5, 18, 18.5, 19, 19.5, 20, etc., and the specific point values ​​in (1-2) can be selected as 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be listed here one by one.

[0019] Preferably, the fermentation suspension comprises, by mass percentage, 0.5-1% sodium alginate, 0.5-0.8% pectin, 0.3-0.6% lecithin, 0.5-1% chitosan and water.

[0020] The mass percentage of the sodium alginate can be selected from 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, etc., the mass percentage of pectin can be selected from 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, etc., the mass percentage of lecithin can be selected from 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, etc., the mass percentage of chitosan can be selected from 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%, 0.95%, 1%, etc., and other specific point values ​​within the above numerical range can be selected, which will not be repeated here one by one.

[0021] Preferably, the fermentation medium comprises, by mass percentage, 1-3% peptone, 1-3% yeast extract, 1-3% wort, 0.02-0.05% potassium dihydrogen phosphate, 0.02-0.05% dipotassium hydrogen phosphate, 0.4-0.8% ammonium sulfate, 0.06-0.1% magnesium sulfate, 0.02-0.05% sodium chloride and water.

[0022] The mass percentage of the peptone can be selected from 1%, 1.2%, 1.4%, 1.6%, 1.8%, 2%, 2.2%, 2.4%, 2.6%, 2.8%, 3% and the like; the mass percentage of the yeast extract can be selected from 1%, 1.2%, 1.4%, 1.6%, 1.8%, 2%, 2.2%, 2.4%, 2.6%, 2.8%, 3% and the like; the mass percentage of the wort can be selected from 1%, 1.2%, 1.4%, 1.6%, 1.8%, 2%, 2.2%, 2.4%, 2.6%, 2.8%, 3% and the like; the mass percentage of the potassium dihydrogen phosphate can be selected from 0.02%, 0.025%, 0.03%, 0.035%, 0.04%, 0.045%, 0.05% and the like; the mass percentage of the potassium dihydrogen phosphate can be selected from 0.03%, 0.025%, 0.03%, 0.035%, 0.04%, 0.045%, 0.05% and the like; The mass percentage of ammonium sulfate can be selected from 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, etc. The mass percentage of magnesium sulfate can be selected from 0.06%, 0.065%, 0.07%, 0.075%, 0.08%, 0.085%, 0.09%, 0.095%, 0.1%, etc. The mass percentage of sodium chloride can be selected from 0.02%, 0.025%, 0.03%, 0.035%, 0.04%, 0.045%, 0.05%, etc. Other specific point values ​​within the above numerical range can be selected, which will not be repeated here.

[0023] Preferably, the fermentation temperature is 28-30°C and the fermentation time is 48-96h.

[0024] The temperature can be selected as 28°C, 28.2°C, 28.4°C, 28.6°C, 28.8°C, 29°C, 29.2°C, 29.4°C, 29.6°C, 29.8°C, 30°C, etc., and the time can be selected as 48h, 52h, 56h, 60h, 64h, 68h, 72h, 76h, 80h, 84h, 88h, 92h, 96h, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be described one by one here.

[0025] Preferably, the fermentation ventilation volume is 0.3-0.6m 3 / h, stirring speed is 180-200rpm.

[0026] The ventilation volume can be selected as 0.3m 3 / h, 0.35m 3 / h、0.4m 3 / h、0.45m 3 / h、0.5m 3 / h、0.55m3 / h、0.6m 3 / h, etc. Other specific point values ​​within the above numerical range can be selected and will not be described here one by one.

[0027] Preferably, the spray drying is carried out at a temperature of 180-220° C., a pressure of 0.3-0.5 MPa, and a time of 6-12 h.

[0028] The temperature can be selected as 180℃, 185℃, 190℃, 195℃, 200℃, 205℃, 210℃, 215℃, 220℃, etc. The pressure can be selected as 0.3MPa, 0.32MPa, 0.34MPa, 0.36MPa, 0.38MPa, 0.4MPa, 0.42MPa, 0.44MPa, 0.46MPa, 0.48MPa, 0.5MPa, etc. The time can be selected as 6h, 6.5h, 7h, 7.5h, 8h, 8.5h, 9h, 9.5h, 10h, 10.5h, 11h, 11.5h, 12h, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be elaborated here one by one.

[0029] In a second aspect, the present invention provides sunscreen microspheres prepared according to the method for preparing sunscreen microspheres with biological activity described in the first aspect.

[0030] In a third aspect, the present invention provides a use of the sunscreen microspheres according to the second aspect in preparing a product with sunscreen efficacy.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] (1) The bioactive sunscreen microspheres prepared by the method described in the present application, the titanium dioxide-zinc oxide mixture can evenly wrap the yeast fermentation product, the product is biologically fermented, has good environmental protection, is easy to apply and absorb, and is mild and non-irritating to the skin.

[0033] (2) Titanium dioxide-zinc oxide mixture as a physical sunscreen can reflect and scatter part of the ultraviolet rays, while yeast fermentation products as biological whitening agents have antioxidant and anti-free radical effects, which can reduce the photoaging damage of the skin caused by ultraviolet radiation, and take into account whitening while protecting the skin from the sun.

[0034] (3) The product is spray dried, and the appropriate temperature and pressure are selected. The atomized microspheres are evenly distributed and stable and are not easy to disperse.

[0035] (4) The sunscreen microspheres obtained through fermentation are not prone to whitening and agglomeration when applied, and can slowly release the active ingredients of yeast fermentation products, prolonging the duration of action. DETAILED DESCRIPTION

[0036] In order to further explain the technical means and effects adopted by the present invention, the technical solution of the present invention is further described below in conjunction with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.

[0037] The sources of the functional ingredients contained in the products involved in the following embodiments and comparative examples are as follows (only the functional ingredients are reflected, and the necessary auxiliary ingredients contained in other commercially available raw materials are not repeated):

[0038] The cerevisiae yeast was cerevisiae ATCC9763.

[0039] Sodium alginate was purchased from Tianjin Dengfeng Chemical Reagent Factory under the trade name of Sodium Alginate Analytical Grade.

[0040] Pectin was purchased from Hainan Zhongchen Biotechnology Co., Ltd. under the trade name of food grade pectin.

[0041] Lecithin was purchased from Maclean Company under the trade name of soy lecithin.

[0042] Chitosan was purchased from Sinopharm Chemical Reagent Co., Ltd. under the trade name of chitosan biochemical reagent.

[0043] The fermentation medium includes, by mass percentage, 1% peptone, 1% yeast extract, 1% malt extract, 0.04% potassium dihydrogen phosphate, 0.04% dipotassium hydrogen phosphate, 0.5% ammonium sulfate, 0.08% magnesium sulfate, 0.03% sodium chloride and the balance water, and is sterilized at 121° C. for 20 min.

[0044] Preparation Example 1

[0045] This preparation example provides a fermentation suspension, which includes 1% sodium alginate, 0.5% pectin, 0.3% lecithin, 1% chitosan and the balance water.

[0046] The preparation method is as follows: the raw materials are mixed at 80° C. and cooled to room temperature to obtain the product.

[0047] Preparation Example 2

[0048] This preparation example provides a fermentation suspension, which includes 0.5% sodium alginate, 0.8% pectin, 0.4% lecithin, 0.8% chitosan and the balance water.

[0049] The preparation method is similar to that of Preparation Example 1.

[0050] Preparation Example 3

[0051] This preparation example provides a fermentation suspension, which includes 0.8% sodium alginate, 0.6% pectin, 0.6% lecithin, 0.5% chitosan and the balance water.

[0052] The preparation method is similar to that of Preparation Example 1.

[0053] Example 1

[0054] This embodiment provides a method for preparing sunscreen microspheres with biological activity, the preparation method comprising:

[0055] (1) mixing titanium dioxide and zinc oxide in a mass ratio of 2:1, and grinding in a sand mill for 20 min to obtain a titanium dioxide-zinc oxide mixture;

[0056] (2) The titanium dioxide-zinc oxide mixture, the fermentation medium, and the fermentation suspension described in Preparation Example 1 were mixed in a volume ratio of 10:1:1, and the viable count of 8% was 1×10 9 CFU / mL of Saccharomyces cerevisiae, fermented at 29°C for 60 h, with aeration of 0.4 m 3 / h, the stirring speed is 190rpm, and a suspension is obtained;

[0057] (3) The suspension is spray dried at a temperature of 200° C., a pressure of 0.4 MPa, and a time of 9 h to obtain the product.

[0058] Example 2

[0059] This embodiment provides a method for preparing sunscreen microspheres with biological activity, the preparation method comprising:

[0060] (1) mixing titanium dioxide and zinc oxide in a mass ratio of 1:1, and grinding them in a sand mill for 20 minutes to obtain a titanium dioxide-zinc oxide mixture;

[0061] (2) The titanium dioxide-zinc oxide mixture, the fermentation medium, and the fermentation suspension described in Preparation Example 2 were mixed in a volume ratio of 20:1:1, and the viable count of 5% inoculated was 5×10 9 CFU / mL of Saccharomyces cerevisiae, fermented at 28°C for 96 h, with an aeration rate of 0.3 m 3 / h, the stirring speed is 180rpm, and a suspension is obtained;

[0062] (3) The suspension is spray dried at a temperature of 220° C., a pressure of 0.5 MPa, and a time of 6 h to obtain the product.

[0063] Example 3

[0064] This embodiment provides a method for preparing sunscreen microspheres with biological activity, the preparation method comprising:

[0065] (1) titanium dioxide and zinc oxide were mixed in a ratio of 5:1, and ground in a sand mill for 20 min to obtain a titanium dioxide-zinc oxide mixture;

[0066] (2) The titanium dioxide-zinc oxide mixture, the fermentation medium, and the fermentation suspension described in Preparation Example 3 were mixed in a volume ratio of 5:1:1, and the viable count of 10% was inoculated with 1×10 9 CFU / mL of Saccharomyces cerevisiae, fermented at 30°C for 48 h, with aeration of 0.6 m 3 / h, the stirring speed is 200rpm, and a suspension is obtained;

[0067] (3) The suspension is spray dried at a temperature of 180° C., a pressure of 0.3 MPa, and a time of 12 h to obtain the product.

[0068] Example 4

[0069] This embodiment provides a method for preparing sunscreen microspheres with biological activity, which is different from Example 1 only in that the number of live bacteria such as Saccharomyces cerevisiae is replaced by Saccharomyces cerevisiae CICC 33188, and other operations remain unchanged.

[0070] Example 5

[0071] This embodiment provides a method for preparing sunscreen microspheres with biological activity, which differs from embodiment 1 only in that step (3) is "spray drying the suspension at a temperature of 200° C., a pressure of 0.1 MPa, and a time of 9 h to obtain the microspheres", and other operations remain unchanged.

[0072] Example 6

[0073] This embodiment provides a method for preparing sunscreen microspheres with biological activity, which differs from embodiment 1 only in that step (3) is "spray drying the suspension at a temperature of 200° C., a pressure of 0.8 MPa, and a time of 9 h to obtain the microspheres", and other operations remain unchanged.

[0074] Comparative Example 1

[0075] This comparative example provides a method for preparing a titanium dioxide-zinc oxide mixture, the preparation method comprising: mixing titanium dioxide and zinc oxide in a mass ratio of 2:1, and grinding in a sand mill for 20 minutes to obtain a titanium dioxide-zinc oxide mixture.

[0076] Comparative Example 2

[0077] This comparative example provides a method for preparing a yeast fermentation product, the preparation method comprising:

[0078] The fermentation medium was inoculated with 8% viable bacteria with a count of 1×10 9 CFU / mL of Saccharomyces cerevisiae, fermented at 29°C for 60 h, with aeration of 0.4 m 3 / h, stirring speed is 190rpm, and the result is obtained.

[0079] Comparative Example 3

[0080] This comparative example provides a method for preparing a sunscreen mixture, which differs from Example 1 only in that step (3) is "placing the suspension in a drying oven for high-temperature drying at 200° C. for 9 hours, and crushing after drying to obtain the mixture", and other operations remain unchanged.

[0081] Comparative Example 4

[0082] This comparative example provides a method for preparing sunscreen microspheres with biological activity, the preparation method comprising:

[0083] (1) mixing titanium dioxide and zinc oxide in a mass ratio of 2:1, and grinding in a sand mill for 20 min to obtain a titanium dioxide-zinc oxide mixture;

[0084] (2) The fermentation medium and the fermentation suspension prepared in Example 1 were mixed at a volume ratio of 1:1 and inoculated with 8% viable bacteria of 1×10 9 CFU / mL of Saccharomyces cerevisiae, fermented at 29°C for 60 h, with aeration of 0.4 m 3 / h, the stirring speed is 190rpm, and a suspension is obtained;

[0085] (3) The titanium dioxide-zinc oxide mixture and the suspension are mixed in a volume ratio of 5:1, and spray-dried at a temperature of 200° C., a pressure of 0.4 MPa, and a time of 9 h to obtain the product.

[0086] Test Example 1

[0087] 1. Subjects: A total of 100 subjects, aged 24 to 42 years old, who met the voluntary inclusion criteria, were randomly divided into groups, with 10 subjects in each group.

[0088] 2. Light source: Daylight simulator xenon arc lamp, all performance indicators meet the measurement specification requirements.

[0089] 3. Test method: Test in accordance with the specific requirements of the currently valid technical specifications. The subject is in a prone position and the back is irradiated. The minimum erythema dose (MED value) of the subject's skin to ultraviolet radiation is predicted 24 hours before the test, and the ultraviolet radiation dose is adjusted according to the predicted results for testing the object being tested.

[0090] On the day of the test, a spot no smaller than 30 cm is selected on the back of the subject. 2 For normal skin area, 2.00±0.05mg / cm 2The test object or reference substance is evenly applied to the above-mentioned area with a dosage of 500 mg / kg, and then the irradiation dose is selected according to the specification requirements. The irradiation is carried out in two situations: ① The test object is not applied to the subject's skin; ② The test object is applied. The experimental results are observed after 24 hours, and the MED values ​​of the two situations are recorded respectively.

[0091] 4. SPF value calculation method:

[0092] SPF = MED value for protected skin / MED value for unprotected skin;

[0093] The individual SPF value is required to be accurate to one decimal place. The arithmetic mean of the SPF values ​​of all subjects protected by the measured object is calculated, and the integer part is the SPF value of the measured sample. The sampling error of the estimated mean can be used to calculate the standard deviation and standard error of the data set. The 95% confidence interval (95% CI) of the mean is required to not exceed 17% of the mean, otherwise the number of subjects should be increased (not more than 25) until the above requirements are met.

[0094] SPF (Sun Protection Factor) is a specific numerical value that indicates the ability of a product to protect against UVB rays. It is an indicator for evaluating the ability of sunscreen cosmetics to protect the skin from sunburn / sunburn. The larger the SPF value, the better the effect of preventing sunburn / sunburn.

[0095] Table 1

[0096]

[0097]

[0098] As can be seen from the data in Table 1, the sunscreen microspheres obtained in the present application have a good sunscreen effect, among which the effect of the fermentation product of Saccharomyces cerevisiae is better than that of other yeast fermentation products, and the drying method and spray drying pressure also affect the sunscreen effect. The sunscreen effect of the microsphere form is better than that of the yeast fermentation product alone and the mixture of titanium dioxide and zinc oxide, and the preparation method also affects the final sunscreen effect.

[0099] Test Example 2

[0100] The test method is as follows:

[0101] 1. Subjects: A total of 100 subjects, aged 24 to 32 years old, who met the voluntary inclusion criteria, were randomly divided into groups, with 10 subjects in each group.

[0102] 2. Light source: Daylight simulator xenon arc lamp, all performance indicators meet the measurement specification requirements.

[0103] 3. Test method: Test in accordance with the specific requirements of the currently valid technical specifications. The subject lies prone and the back is exposed. The minimum blackening amount (MPPD value) of the subject's skin to ultraviolet radiation is predicted 24 hours before the test, and the ultraviolet radiation amount is adjusted according to the predicted results for testing the object. The test first selects a spot no less than 30cm on the subject's back. 2 For normal skin area, (2.00±0.05)mg / cm 2 Apply the test object or reference product evenly on the above area with the dosage; then select the UVA irradiation amount according to the specification requirements, and irradiate in two situations: ① The test object is not applied to the subject's skin; ② The test object is applied. Observe the experimental results after 24 hours and record the MPPD values ​​of the two situations respectively.

[0104] 4. Calculation method of PFA value:

[0105] PFA = MPPD value of protected skin / MPPD value of unprotected skin;

[0106] The individual PFA value is required to be accurate to one decimal place. The arithmetic mean of the PFA values ​​of all subjects protected by the measured object is calculated, and the integer part is the PFA value of the measured sample.

[0107] PFA (protection factor of UVA) is a specific value that indicates the ability of a product to protect against long-wave ultraviolet rays UVA. The larger the PFA value, the better the UVA protection effect.

[0108] Table 2

[0109] Group PFA value Example 1 42 Example 2 40 Example 3 40 Example 4 34 Example 5 35 Example 6 36 Comparative Example 1 29 Comparative Example 2 34 Comparative Example 3 37 Comparative Example 4 36

[0110] As can be seen from the data in Table 2, the sunscreen microspheres obtained in the present application have a good sunscreen effect, among which the effect of the fermentation product of Saccharomyces cerevisiae is better than that of other yeast fermentation products, and the drying method and spray drying pressure also affect the sunscreen effect. The sunscreen effect of the microsphere form is better than that of the yeast fermentation product alone and the mixture of titanium dioxide and zinc oxide, and the preparation method also affects the final sunscreen effect.

[0111] Test Example 3

[0112] Skin feel test

[0113] In order to evaluate the skin feel of the present invention, samples prepared in Examples 1-6 and Comparative Examples 1-4 were selected as test samples for skin feel evaluation. 100 women aged 25 to 35 (who passed the sensory test training) were selected for product sensory evaluation test, 10 people in each group, in an independent environment with constant temperature (22±1°C) and relative humidity (50±5%), and the test was conducted after resting for 1 hour. The scoring system: the score is 1 to 10 points, and the higher the score, the stronger the characteristic of the indicator of the project.

[0114] Table 3

[0115] Group Moisture Greasy feeling Makeup Example 1 8.8 1.2 1.3 Example 2 7.5 1.6 2.2 Example 3 7.7 1.8 1.9 Example 4 6.5 2.2 2.8 Example 5 6.4 3.8 2.2 Example 6 6.5 2.9 2.8 Comparative Example 1 2.0 5.4 5.8 Comparative Example 2 8.1 1.9 1.5 Comparative Example 3 5.1 4.8 4.5 Comparative Example 4 5.9 5.8 5.4

[0116] From the data in Table 3, it can be seen that the sunscreen microspheres obtained in this application have a good skin feel, which is moist and non-greasy, and does not have a strong makeup feeling or whitening. The selection of yeast, drying method, preparation method, etc. will also affect the above effects.

[0117] Test Example 4

[0118] Irritation test

[0119] The samples prepared in Examples 1-6 were subjected to patch tests to detect their potential to cause adverse reactions on human skin.

[0120] The test was conducted in accordance with the human skin patch test method in the "Technical Specifications for Safety of Cosmetics" (2015 edition), and 30 volunteers aged 18 to 60 who met the test requirements were selected as subjects (15 males and 15 females). Each sample was added to the patch tester at a dosage of 0.020 to 0.025 g, and no substance was added to the blank control. The patch tester was applied to the flexion side of the subject's forearm with a non-irritating tape, and gently pressed with the palm of the hand to evenly apply it to the skin. The test site was marked for observation, and applied once every 24 hours. After 30 minutes after the patch was removed, the skin reaction was observed after the indentation disappeared. If it was a suspicious reaction or a positive reaction, the subject stopped the patch test; if it was a negative reaction, the patch test was continued at the same test site of the subject, and the patch test was repeated 6 times in total, and the reaction results of the test group were recorded.

[0121] Table 4

[0122] grade symbol Identification criteria 0 - Negative reaction: no irritation, no erythema 1 ± Suspected reaction: Mild erythema 2 + Weak positive reaction: erythema 3 ++ Strong positive reaction: erythema, papules, blisters 4 +++ Very strong positive reaction: severe edema, large blisters

[0123] Table 5

[0124] 1 2 3 4 5 6 Example 1 0 0 0 0 0 0 Example 2 0 0 0 0 0 0 Example 3 0 0 0 0 0 0 Example 4 0 0 0 0 0 0 Example 5 0 0 0 0 0 0 Example 6 0 0 0 0 0 0

[0125] It can be seen from the data in Table 5 that the microspheres obtained in the present application are non-irritating and will not cause allergic reactions.

[0126] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the preparation method of the bioactive sunscreen microspheres and its products and applications, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0127] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0128] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A method for preparing bioactive sunscreen microspheres, characterized in that: The preparation method comprises: (1) mixing titanium dioxide and zinc oxide to obtain a first mixture; (2) inoculating the yeast strain into a fermentation medium, mixing and fermenting the mixture with the first mixture and a fermentation suspension to obtain a suspension; (3) Spray-dry the suspension to obtain the product.

2. The method for preparing the bioactive sunscreen microspheres according to claim 1, characterized in that: The mass ratio of titanium dioxide to zinc oxide is (5-10):(2-5); Preferably, the yeast inoculation amount is 5-10%, and the viable bacteria count is 1×10 9 CFU / mL-1×10 10 CFU / mL; Preferably, the yeast comprises Saccharomyces cerevisiae.

3. The method for preparing the bioactive sunscreen microspheres according to claim 1 or 2, characterized in that: The volume ratio of the fermentation medium, the first mixture and the fermentation suspension is (10-20):(1-2):(1-2).

4. The method for preparing the bioactive sunscreen microspheres according to any one of claims 1 to 3, characterized in that: The fermentation suspension comprises, by weight percentage, 0.5-1% sodium alginate, 0.5-0.8% pectin, 0.3-0.6% lecithin, 0.5-1% chitosan and water.

5. The method for preparing the bioactive sunscreen microspheres according to any one of claims 1 to 4, characterized in that: The fermentation medium comprises, by mass percentage, 1-3% peptone, 1-3% yeast extract, 1-3% malt extract, 0.02-0.05% potassium dihydrogen phosphate, 0.02-0.05% dipotassium hydrogen phosphate, 0.4-0.8% ammonium sulfate, 0.06-0.1% magnesium sulfate, 0.02-0.05% sodium chloride and water.

6. The method for preparing the bioactive sunscreen microspheres according to any one of claims 1 to 5, characterized in that: The fermentation temperature is 28-30°C and the fermentation time is 48-96h.

7. The method for preparing the bioactive sunscreen microspheres according to any one of claims 1 to 6, characterized in that: The fermentation ventilation volume is 0.3-0.6m 3 / h, stirring speed is 180-200rpm.

8. The method for preparing the bioactive sunscreen microspheres according to any one of claims 1 to 7, characterized in that: The spray drying temperature is 180-220° C., the pressure is 0.3-0.5 MPa, and the time is 6-12 hours.

9. Sunscreen microspheres prepared by the method for preparing sunscreen microspheres with biological activity according to any one of claims 1 to 8.

10. Use of the sunscreen microspheres according to claim 9 in preparing products with sunscreen efficacy.

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