Preparation method of active titanium dioxide as well as product and application of active titanium dioxide

Abstract

The invention relates to a preparation method of active titanium dioxide as well as a product and application of the active titanium dioxide. The preparation method comprises the following steps: mixing cistanche with water, and carrying out ultrasonic extraction to obtain an extracting solution; inoculating lactobacillus rhamnosus and lactobacillus plantarum into the sterilized extracting solution, and fermenting to obtain a first fermentation product; inoculating the first fermentation product with filmed saccharomyces fibuligerus, and fermenting to obtain a second fermentation product; and centrifuging and filtering the second fermentation product, mixing the supernatant with titanium dioxide, homogenizing, and freeze-drying to obtain the product. According to the invention, two sunscreen synergistic components with different action mechanisms are selected in a targeted manner, so that the effects of rapid film forming and lasting hair loss prevention are achieved, meanwhile, the sunscreen value is increased, and the use of other chemical sunscreen agents is reduced.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics and relates to a preparation method of active titanium dioxide and a product and application thereof. Background Art

[0002] Ultraviolet rays are an important external physical factor that affects the biological effects of the skin. They can cause the proliferation or apoptosis of melanocytes and increase pigment synthesis. Among them, UVA (320-400) can penetrate the skin and reach the dermis, which is the main cause of skin aging; UVB (280-320) mainly damages the epidermis of the skin, causing skin peeling, pigmentation, etc. Currently, sunscreens on the market are divided into physical sunscreens and chemical sunscreens. Physical sunscreens mainly reflect ultraviolet rays to achieve the purpose of sun protection; chemical sunscreens mainly use chemical ingredients to absorb ultraviolet rays for sun protection. However, they all have disadvantages such as being greasy, difficult to form a film, not waterproof and easy to fall off.

[0003] Cistanche deserticola was first recorded in Shennong's Herbal Classic. It is a traditional precious medicinal material in my country and is known as the "desert ginseng". It is listed as a top-grade product. The functions and indications of Cistanche deserticola are to tonify kidney yang, benefit essence and blood, and moisten the intestines and promote bowel movements. Modern research shows that Cistanche deserticola contains a variety of bioactive substances such as phenylethanol glycosides, iridoid ether terpenoid glycosides, polysaccharides, and alkaloids. Among them, phenylethanol glycosides include echinacoside and verbascoside, which have strong absorption at 280-380nm and can be used as a natural sunscreen to alleviate the damage of ultraviolet rays to the skin.

[0004] Titanium dioxide has excellent hiding power and can cover facial pigmentation and spots. It can also reflect light to make the skin brighter. Therefore, adding titanium dioxide to some skin-lightening products can help improve skin tone. Titanium dioxide can absorb oil on the surface of the skin and has a good oil control effect on greasy skin. Titanium dioxide is a highly stable skin care ingredient that can maintain good stability under various environmental conditions. This stability makes titanium dioxide skin care products more durable and effective. Titanium dioxide is a physical sunscreen that forms a physical film on the skin surface to reflect and scatter ultraviolet rays to prevent ultraviolet rays from damaging the skin. Therefore, titanium dioxide skin care products can have a good sun protection effect.

[0005] Consumers want sunscreen products to maintain high UV protection while also being durable, stable, whitening and safe. Therefore, there is an urgent need to provide a sunscreen product that is whitening, safe and durable. Summary of the invention

[0006] In view of the deficiencies of the prior art, the object of the present invention is to provide a method for preparing active titanium dioxide and its product and application.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a method for preparing active titanium dioxide, the preparation method comprising:

[0009] (1) mixing Cistanche deserticola with water and performing ultrasonic extraction to obtain an extract;

[0010] (2) inoculating Lactobacillus rhamnosus and Lactobacillus plantarum into the sterilized extract, and fermenting to obtain a first fermentation product;

[0011] (3) inoculating the capsule-coated yeast into the first fermentation product, fermenting, and obtaining a second fermentation product;

[0012] (4) The second fermentation product is centrifuged, filtered, and the supernatant is mixed with titanium dioxide, homogenized, and freeze-dried to obtain the product.

[0013] The present invention achieves the effects of rapid film formation and long-lasting sunscreen protection by selectively selecting two sunscreen synergistic components with different action mechanisms, while improving the sunscreen value and reducing the use of other chemical sunscreens. The Cistanche deserticola provided by the present invention is fermented to greatly increase the content and efficacy of its active ingredients, and freeze-drying technology is used to retain its biological activity to the maximum extent, avoiding the problem of its activity reduction due to high temperature.

[0014] Preferably, the mass ratio of the Cistanche deserticola to water is 1:(5-10), wherein the specific point values ​​in (5-10) can be selected from 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be repeated here.

[0015] Preferably, the power of the ultrasound is 450-550W, and the time is 25-45min.

[0016] The power of the ultrasound can be selected as 450W, 460W, 470W, 480W, 490W, 500W, 510W, 520W, 530W, 540W, 550W, etc., and the time can be selected as 25min, 28min, 30min, 32min, 35min, 38min, 40min, 42min, 45min, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be described one by one here.

[0017] Preferably, step (1) further comprises mixing the extract with nutrients and sterilizing.

[0018] Preferably, the sterilization temperature is 85-90°C and the time is 20-40 minutes.

[0019] The temperature can be selected as 85°C, 86°C, 87°C, 88°C, 89°C, 90°C, etc., and the time can be selected as 20min, 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min, 38min, 40min, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be elaborated here.

[0020] Preferably, the nutrients include glucose and peptone.

[0021] Preferably, the mass percentage of glucose in the sterilized extract is 0.3-0.6%, and the mass percentage of peptone is 0.7-1.5%.

[0022] The mass percentage of the glucose can be selected from 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6% and the like, and the mass percentage of the peptone can be selected from 0.7%, 0.8%, 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5% and the like. Other specific point values ​​within the above numerical range can be selected and will not be described one by one here.

[0023] Preferably, the viable count of Lactobacillus rhamnosus is 4×10 9 CFU / g-8×10 9 CFU / g, the inoculum size was 3-6%.

[0024] The viable count can be selected as 4×10 9 CFU / g, 4.2×10 9 CFU / g, 4.5×10 9 CFU / g, 4.8×10 9 CFU / g, 5×10 9 CFU / g, 5.2×10 9 CFU / g, 5.5×10 9 CFU / g, 5.8×10 9 CFU / g, 6×10 9 CFU / g, 6.2×10 9 CFU / g, 6.5×10 9 CFU / g, 6.8×10 9 CFU / g, 7×10 9 CFU / g, 7.2×10 9 CFU / g, 7.5×10 9 CFU / g, 7.8×10 9 CFU / g, 8×10 9CFU / g, etc. The inoculation amount can be selected from 3%, 3.2%, 3.5%, 3.8%, 4%, 4.2%, 4.5%, 4.8%, 5%, 5.2%, 5.5%, 5.8%, 6%, etc. Other specific points within the above numerical range can be selected, so they will not be elaborated here.

[0025] Preferably, the viable count of the plant lactobacillus is 4×10 9 CFU / g-8×10 9 CFU / g, the inoculation amount is 2-5%.

[0026] The viable count can be selected as 4×10 9 CFU / g, 4.2×10 9 CFU / g, 4.5×10 9 CFU / g, 4.8×10 9 CFU / g, 5×10 9 CFU / g, 5.2×10 9 CFU / g, 5.5×10 9 CFU / g, 5.8×10 9 CFU / g, 6×10 9 CFU / g, 6.2×10 9 CFU / g, 6.5×10 9 CFU / g, 6.8×10 9 CFU / g, 7×10 9 CFU / g, 7.2×10 9 CFU / g, 7.5×10 9 CFU / g, 7.8×10 9 CFU / g, 8×10 9 CFU / g, etc. The inoculation amount can be selected as 2%, 2.2%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.8%, 4%, 4.2%, 4.5%, 4.8%, 5%, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be listed here one by one.

[0027] Preferably, the viable count of the capsule-coated yeast is 4×10 9 CFU / g-8×10 9 CFU / g, the inoculum size was 4-6%.

[0028] The viable count can be selected as 4×10 9 CFU / g, 4.2×10 9 CFU / g, 4.5×10 9 CFU / g, 4.8×10 9 CFU / g, 5×10 9 CFU / g, 5.2×109 CFU / g, 5.5×10 9 CFU / g, 5.8×10 9 CFU / g, 6×10 9 CFU / g, 6.2×10 9 CFU / g, 6.5×10 9 CFU / g, 6.8×10 9 CFU / g, 7×10 9 CFU / g, 7.2×10 9 CFU / g, 7.5×10 9 CFU / g, 7.8×10 9 CFU / g, 8×10 9 CFU / g, etc. The inoculation amount can be selected as 4%, 4.2%, 4.5%, 4.8%, 5%, 5.2%, 5.5%, 5.8%, 6%, etc. Other specific points within the above numerical range can be selected, and they will not be described here one by one.

[0029] Preferably, the fermentation temperature in step (2) is 30-35°C, the fermentation time is 6-10 hours, and the pH is 4.5-9.5.

[0030] The temperature can be selected as 30℃, 31℃, 32℃, 33℃, 34℃, 35℃, etc. The time can be selected as 6h, 6.2h, 6.5h, 6.8h, 7h, 7.2h, 7.5h, 7.8h, 8h, 8.2h, 8.5h, 8.8h, 9h, 9.2h, 9.5h, 9.8h, 10h, etc. The pH can be selected as 4.5, 4.8, 5, 5.2, 5.5, 5.8, 6, 6.2, 6.5, 6.8, 7, 7.2, 7.5, 8, 8.2, 8.5, 8.8, 9, 9.2, 9.5, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be elaborated here.

[0031] Preferably, the fermentation temperature in step (3) is 28-30°C, the fermentation time is 18-30h, and the pH is 4-8.

[0032] The temperature can be selected as 28℃, 28.2℃, 28.5℃, 28.8℃, 29℃, 29.2℃, 29.5℃, 29.8℃, 30℃, etc. The time can be selected as 18h, 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h, 29h, 30h, etc. The pH can be selected as 4, 4.2, 4.5, 4.8, 5, 5.2, 5.5, 5.8, 6, 6.2, 6.5, 6.8, 7, 7.2, 7.5, 7.8, 8, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be elaborated here.

[0033] Preferably, the centrifugal speed in step (4) is 3000-5000 rpm and the time is 25-35 min.

[0034] The centrifugal speed can be selected as 3000rpm, 3200rpm, 3400rpm, 3600rpm, 3800rpm, 4000rpm, 4200rpm, 4400rpm, 4600rpm, 4800rpm, 5000rpm, etc., and the time can be selected as 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35min, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be described one by one here.

[0035] Preferably, in step (4), the mass ratio of the supernatant to the titanium dioxide is 25:(1-2), wherein the specific point values ​​in (1-2) can be selected from 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, etc., and other specific point values ​​within the above numerical range can be selected, which will not be repeated here.

[0036] Preferably, the homogenization method is high-pressure microjet homogenization, and the homogenization pressure is 90-160MPa, for example, 90MPa, 100MPa, 110MPa, 120MPa, 130MPa, 140MPa, 150MPa, 160MPa, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be described one by one here.

[0037] Preferably, the particle size of the active titanium dioxide is 50-120nm, for example, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, 105nm, 110nm, 115nm, 120nm, etc. Other specific point values ​​within the above numerical range can be selected, which will not be described here one by one.

[0038] In a second aspect, the present invention provides an active titanium dioxide prepared according to the method for preparing active titanium dioxide described in the first aspect.

[0039] In a third aspect, the present invention provides a use of the active titanium dioxide according to the second aspect in the preparation of a sunscreen product.

[0040] Preferably, the mass percentage of active titanium dioxide in the sunscreen product is 10-20%, for example 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, etc. Other specific points within the above numerical range can be selected and will not be described here one by one.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] 1. The present invention uses a specific sunscreen combination. Titanium dioxide as a physical sunscreen can not only form a sunscreen film on the skin surface, but also absorb the grease on the skin surface. Even if the skin is oily, it will not fall off easily, resulting in reduced sunscreen effect. The phenylethanol glycosides in Cistanche deserticola have strong whitening and anti-aging effects, and also have the function of absorbing ultraviolet rays. It is a sunscreen with biological activity. After microbial fermentation, the whitening and sunscreening ability of the obtained fermentation liquid is doubled.

[0043] 2. Inorganic whitening sunscreen agents are combined with plant whitening active substances. Titanium dioxide can form a physical sunscreen film on the skin surface through the compounding of titanium dioxide and fermented Cistanche deserticola extract, and the fermented Cistanche deserticola broth not only enhances the absorption of ultraviolet rays, but also inhibits the production of melanin to prevent the skin from darkening after exposure. The sunscreen composition prepared by the present invention has excellent sunscreen effect and good anti-UV function.

[0044] 3. The preparation of the active titanium dioxide provided by the present invention is carried out through two-step fermentation. In the first step of fermentation, the phenylethanol glycoside active substances in the Cistanche deserticola extract are first decomposed into small molecules of verbascoside and echinacoside, etc., while utilizing the polysaccharides and other components in Cistanche deserticola and secreting some small molecule active substances; the second step of fermentation increases the content of the active ingredients in the fermentation liquid.

[0045] 4. Titanium dioxide has high stability and maintains good stability under various environmental conditions. The compound product after the composition is homogenized by high-pressure microfluidization has good stability, mildness, no irritation, and good feel in use.

[0046] 5. The sunscreen composition provided by the present invention is finally freeze-dried to form a finished product, thereby retaining the biological activity of the fermentation extract to the greatest extent. DETAILED DESCRIPTION

[0047] 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.

[0048] 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):

[0049] Titanium dioxide: titanium dioxide content ≥98%; aluminum oxide / silicon dioxide content ≤2%.

[0050] Preparation Example 1

[0051] This preparation example provides a method for preparing Lactobacillus rhamnosus cells, the preparation method comprising:

[0052] The Lactobacillus rhamnosus CICC 22151 strain was inoculated into a YPD medium and cultured at 30°C for 16 hours to obtain a primary seed solution, and the primary seed solution was transferred to a YPD medium at an inoculation rate of 10%, and cultured at 30°C for 28 hours to obtain a secondary seed solution. The secondary seed solution was centrifuged at 5000 rpm for 10 minutes, and the supernatant was discarded to obtain the secondary seed solution.

[0053] Preparation Example 2

[0054] This preparation example provides a method for preparing Lactobacillus plantarum, the preparation method comprising:

[0055] The plant lactobacillus CICC 20265 strain was inoculated into a YPD medium and cultured at 30°C for 16 hours to obtain a primary seed solution, and the primary seed solution was transferred to a YPD medium at an inoculation rate of 10%, and cultured at 30°C for 28 hours to obtain a secondary seed solution. The secondary seed solution was centrifuged at 5000 rpm for 10 minutes, and the supernatant was discarded to obtain the secondary seed solution.

[0056] Preparation Example 3

[0057] This preparation example provides a method for preparing Lactobacillus plantarum, the preparation method comprising:

[0058] The CICC 33188 strain of the capsule-coated yeast was inoculated into the YPD medium and cultured at 30°C for 16 hours to obtain the primary seed solution, and the primary seed solution was transferred to the YPD medium at an inoculation rate of 10%, and cultured at 30°C for 28 hours to obtain the secondary seed solution. The secondary seed solution was centrifuged at 5000rpm for 10 minutes, and the supernatant was discarded to obtain the secondary seed solution.

[0059] Example 1

[0060] This embodiment provides a method for preparing active titanium dioxide, the preparation method comprising:

[0061] (1) Mix Cistanche deserticola with water in a mass ratio of 1:8, perform ultrasonic extraction at a power of 500 W for 30 min to obtain an extract, add glucose with a final concentration of 0.5% and peptone with a final concentration of 1% to the extract, and sterilize at 90° C. for 30 min;

[0062] (2) The Lactobacillus rhamnosus cells obtained in Preparation Example 1 and the Lactobacillus plantarum cells obtained in Preparation Example 2 were inoculated into the sterilized extract. The number of viable cells of the Lactobacillus rhamnosus cells was 4.9×10 9 CFU / g, the inoculation amount was 4%, and the number of viable Lactobacillus plantarum cells was 4.9×10 9CFU / g, inoculation amount of 3%, fermentation at 34°C for 8h, pH 7, to obtain the first fermentation product;

[0063] (3) The capsule-coated yeast cells obtained in Preparation Example 3 were inoculated into the first fermentation product. The number of viable cells of the capsule-coated yeast cells was 5.4×10 9 CFU / g, inoculation amount of 5%, fermentation at 29°C for 25h, pH 6, to obtain the second fermentation product;

[0064] (4) The second fermentation product is centrifuged at a speed of 4000 rpm for 30 min. After filtration, the supernatant is mixed with titanium dioxide at a mass ratio of 25:1.5. High-pressure microfluidization is performed at a homogenization pressure of 120 MPa, and freeze-dried. The particle size of the obtained titanium dioxide is about 70 nm.

[0065] Example 2

[0066] This embodiment provides a method for preparing active titanium dioxide, the preparation method comprising:

[0067] (1) Mix Cistanche deserticola with water in a mass ratio of 1:5, perform ultrasonic extraction, and use an ultrasonic power of 450 W for 45 min to obtain an extract. Add glucose with a final concentration of 0.3% and peptone with a final concentration of 1.5% to the extract, and sterilize at 90° C. for 30 min.

[0068] (2) The Lactobacillus rhamnosus cells obtained in Preparation Example 1 and the Lactobacillus plantarum cells obtained in Preparation Example 2 were inoculated into the sterilized extract. The number of viable cells of the Lactobacillus rhamnosus cells was 4×10 9 CFU / g, the inoculation amount is 3%, and the number of viable Lactobacillus plantarum cells is 4×10 9 CFU / g, inoculation amount of 2%, fermentation at 30°C for 10h, pH 5, to obtain the first fermentation product;

[0069] (3) The capsule-coated yeast cells obtained in Preparation Example 3 were inoculated into the first fermentation product. The number of viable cells of the capsule-coated yeast cells was 4×10 9 CFU / g, inoculation amount of 4%, fermentation at 28°C for 30h, pH 4, to obtain the second fermentation product;

[0070] (4) The second fermentation product is centrifuged at a speed of 3000 rpm for 35 min. After filtration, the supernatant is mixed with titanium dioxide at a mass ratio of 25:1. High-pressure microfluidization is performed at a homogenization pressure of 90 MPa, and freeze-dried. The particle size of the obtained titanium dioxide is about 50 nm.

[0071] Example 3

[0072] This embodiment provides a method for preparing active titanium dioxide, the preparation method comprising:

[0073] (1) Mix Cistanche deserticola with water in a mass ratio of 1:10, perform ultrasonic extraction at a power of 550 W for 25 min, obtain an extract, add glucose with a final concentration of 0.6% and peptone with a final concentration of 0.7% to the extract, and sterilize at 90° C. for 30 min;

[0074] (2) The Lactobacillus rhamnosus cells obtained in Preparation Example 1 and the Lactobacillus plantarum cells obtained in Preparation Example 2 were inoculated into the sterilized extract. The number of viable cells of the Lactobacillus rhamnosus cells was 8×10 9 CFU / g, the inoculation amount is 6%, and the number of viable Lactobacillus plantarum cells is 8×10 9 CFU / g, inoculation amount of 5%, fermentation at 35°C for 6h, pH 9, to obtain the first fermentation product;

[0075] (3) The capsule-coated yeast cells obtained in Preparation Example 3 were inoculated into the first fermentation product. The number of viable cells of the capsule-coated yeast cells was 8×10 9 CFU / g, inoculation amount of 6%, fermentation at 30°C for 18h, pH 8, to obtain a second fermentation product;

[0076] (4) The second fermentation product is centrifuged at a speed of 5000 rpm for 25 min. After filtration, the supernatant is mixed with titanium dioxide at a mass ratio of 25:2. High-pressure microfluidization is performed at a homogenization pressure of 160 MPa, and freeze-dried. The particle size of the obtained titanium dioxide is about 120 nm.

[0077] Example 4

[0078] The present embodiment provides a method for preparing active titanium dioxide, which differs from the embodiment 1 only in that step (4) is "centrifuging the second fermentation product at a speed of 4000 rpm for 30 min, filtering and mixing the supernatant with titanium dioxide at a mass ratio of 25:1.5, performing high-pressure homogenization at a homogenization pressure of 20000 psi, freeze-drying, and obtaining a titanium dioxide particle size of about 70 nm", and other operations remain unchanged.

[0079] Comparative Example 1

[0080] This comparative example provides a method for preparing active titanium dioxide, which differs from Example 1 only in that step (2) is "inoculating the Lactobacillus rhamnosus cells obtained in Preparation Example 1 into the sterilized extract, and the number of viable Lactobacillus rhamnosus cells is 4.9×10 9 CFU / g, inoculation amount of 7%, fermentation at 34°C for 8h, pH 7, and obtaining the first fermentation product". Other operations remained unchanged.

[0081] Comparative Example 2

[0082] This comparative example provides a method for preparing active titanium dioxide, which differs from Example 1 only in that step (2) is "inoculating the plant lactobacillus cells obtained in Preparation Example 2 into the sterilized extract, and the number of viable cells of the plant lactobacillus cells is 4.9×10 9 CFU / g, inoculation amount of 7%, fermentation at 34°C for 8h, pH 7, and obtaining the first fermentation product". Other operations remained unchanged.

[0083] Comparative Example 3

[0084] This comparative example provides a method for preparing active titanium dioxide, which differs from Example 1 only in that step (2) is not included, and other operations remain unchanged.

[0085] Comparative Example 4

[0086] This comparative example provides a method for preparing active titanium dioxide, which differs from Example 1 only in that step (3) is not included, and other operations remain unchanged.

[0087] Comparative Example 5

[0088] This comparative example provides a method for preparing active titanium dioxide, which comprises:

[0089] (1) Mix Cistanche deserticola with water in a mass ratio of 1:8, perform ultrasonic extraction at a power of 500 W for 30 min to obtain an extract, add glucose with a final concentration of 0.5% and peptone with a final concentration of 1% to the extract, and sterilize at 90° C. for 30 min;

[0090] (2) The Lactobacillus rhamnosus cells obtained in Preparation Example 1, the Lactobacillus plantarum cells obtained in Preparation Example 2, and the capsule-coated yeast cells obtained in Preparation Example 3 were inoculated into the sterilized extract. The number of viable cells of the Lactobacillus rhamnosus cells was 4.9×10 9 CFU / g, the inoculation amount was 4%, and the number of viable Lactobacillus plantarum cells was 4.9×10 9 CFU / g, the inoculation amount was 3%, and the number of viable bacteria of the capsule-coated yeast was 5.4×10 9 CFU / g, inoculation amount of 5%, fermentation at 29°C for 25h, pH 7, to obtain the first fermentation product;

[0091] (4) The first fermentation product is centrifuged at a speed of 4000 rpm for 30 min. After filtration, the supernatant is mixed with titanium dioxide at a mass ratio of 25:1.5. High-pressure microfluidization is performed at a homogenization pressure of 120 MPa, and freeze-dried. The particle size of the obtained titanium dioxide is about 70 nm.

[0092] Comparative Example 6

[0093] This comparative example provides a method for preparing titanium dioxide, which comprises:

[0094] (1) Mix Cistanche deserticola with water in a mass ratio of 1:8, perform ultrasonic extraction, and use an ultrasonic power of 500 W for 30 min to obtain an extract, and sterilize the extract at 90° C. for 30 min;

[0095] (2) The sterilized extract is centrifuged at a speed of 4000 rpm for 30 min, filtered, and the supernatant is mixed with titanium dioxide at a mass ratio of 25:1.5. High-pressure microfluidization is performed at a homogenization pressure of 120 MPa, and freeze-dried to obtain a titanium dioxide particle size of about 70 nm.

[0096] Application Example 1

[0097] This application example provides a sunscreen lotion, which includes, by mass percentage, 15% of active titanium dioxide obtained in Example 1, 5% of butylene glycol, 0.5% of isopropyl alcohol, 0.05% of disodium EDTA, 0.8% of sodium chloride, 1% of PEG-3 polydimethylsiloxane, 1% of distearyl dimethyl ammonium chloride, 1% of sorbitan sesquioleate, 2% of stearic acid, 6% of triethoxycaprylylsilane, 5% of dextrin palmitate, and the balance of water.

[0098] The preparation method is as follows: butanediol, isopropanol, disodium EDTA, sodium chloride and water are mixed at 80°C to obtain a water phase; PEG-3 polydimethylsiloxane, distearyl dimethyl ammonium chloride, sorbitan sesquioleate, stearic acid, triethoxycaprylylsilane and dextrin palmitate are mixed at 80°C to obtain an oil phase; the water phase and the oil phase are mixed, and after homogenization, the mixture is mixed with active titanium dioxide at 45°C to obtain the product.

[0099] Application Example 2-4

[0100] This application example provides three kinds of sunscreen lotions, which differ from application example 1 only in that an equal amount of the active titanium dioxide obtained in example 1 is replaced by the active titanium dioxide obtained in examples 2-4, and other ingredients and contents remain unchanged.

[0101] The preparation method refers to Application Example 1.

[0102] Comparative Application Examples 1-6

[0103] This comparative application example provides 6 kinds of sunscreen lotions, which differ from application example 1 only in that an equal amount of the active titanium dioxide obtained in example 1 is replaced by the titanium dioxide obtained in comparative examples 1-6, and other ingredients and contents remain unchanged.

[0104] The preparation method refers to Application Example 1.

[0105] Test Example 1

[0106] Contents of Verbascoside and Echinacoside in Fermented Broth of Cistanche deserticola

[0107] Test method:

[0108] Preparation of reference solution: Accurately weigh 0.1540 g of reference echinacoside and 0.0165 g of verbascoside, mix them, add 50% methanol aqueous solution to 100 mL, and fully dissolve them.

[0109] Preparation of the test solution: Take the Cistanche deserticola fermentation broth of Examples 1-3 and Comparative Examples 1-6, and filter through a 0.22 μm filter membrane to obtain the solution.

[0110] Chromatographic conditions: Waters HSS T3 column (100 mm×2.1 mm, 1.8 μm); mobile phase: methanol (A)-0.1% formic acid aqueous solution (B) gradient elution, flow rate 0.3 mL / min; column temperature: 30°C; detection wavelength: 330 nm; injection volume: 1 μL.

[0111] Sample content determination: Take the reference solution and each test solution, inject and test according to the above chromatographic conditions, and calculate the content by external standard method. The results are as follows.

[0112] Table 1

[0113] Echinacoside(%) Verbascoside(%) Example 1 3.15 1.81 Example 2 3.02 1.63 Example 3 3.04 1.58 Comparative Example 1 2.71 1.26 Comparative Example 2 2.56 1.32 Comparative Example 3 2.10 1.08 Comparative Example 4 2.89 1.34 Comparative Example 5 2.16 1.01 Comparative Example 6 1.56 0.74

[0114] The phenylethanol glycoside active substances in the Cistanche extract are decomposed into small molecules of verbascoside and echinacoside, which are the core components of Cistanche. From the data in Table 1, it can be seen that different fermentation methods have a great influence on the content of active substances. The lack of any step in the two-step fermentation or the completion of the two-step fermentation in one step will affect the fermentation effect. In addition, Lactobacillus rhamnosus and Lactobacillus plantarum can cooperate with each other in fermentation. The combined use of the two strains has a better fermentation effect.

[0115] Test Example 2

[0116] Tyrosinase inhibition value

[0117] The whitening performance testing method of the present invention is to verify the inhibitory effect of the whitening composition on melanin through an in vitro tyrosinase inhibition test, and the testing method refers to T / SHRH 015-2018 "Cosmetics-Tyrosinase Activity Inhibition Experimental Method".

[0118] The results are shown in Table 2.

[0119] Table 2

[0120]

[0121]

[0122] As can be seen from the data in Table 2, the titanium dioxide obtained by the present invention has a good inhibitory effect on tyrosinase and a good whitening effect. The lack of any one step in the two-step fermentation or the completion of the two-step fermentation in one step will affect the fermentation effect, and Lactobacillus rhamnosus and Lactobacillus plantarum can cooperate with each other in fermentation. The combined use of the two strains has a better fermentation effect.

[0123] Test Example 3

[0124] Finished product sunscreen SPF value and PFA value

[0125] The sun protection index (SP value) of sunscreen lotion is measured according to the sun protection index (SP value) of sunscreen cosmetics in Chapter 8, Section 2 of the 2015 edition of the "Technical Specifications for Safety of Cosmetics", and the PFA value is measured according to the detection method for the ultraviolet A wave (i.e. UVA) protection index (PFA value) in Chapter 8, Section 4 of the 2015 edition of the "Technical Specifications for Safety of Cosmetics".

[0126] Table 3

[0127] SPF value PFA value Application Example 1 31 33 Application Example 2 25 29 Application Example 3 27 29 Application Example 4 30 31 Comparative application example 1 22 21 Comparative Application Example 2 21 21 Comparative Application Example 3 20 20 Comparative Application Example 4 22 22 Comparative Application Example 5 22 20 Comparative Application Example 6 12 9

[0128] It can be seen from the data in Table 3 that the sunscreen product made from the titanium dioxide obtained in the present invention has a good sunscreen effect. The lack of any one of the two-step fermentation steps or the completion of the two-step fermentation in one step will affect the fermentation effect, and Lactobacillus rhamnosus and Lactobacillus plantarum can cooperate with each other in fermentation. The combined use of the two strains has a better fermentation effect.

[0129] Test Example 4

[0130] Product stability testing

[0131] Refer to GB / T 29665-2013, and use a more stringent standard than GB / T 29665-2013 for stability testing.

[0132] Test content: including heat resistance, cold resistance and centrifugal test.

[0133] Heat resistance test conditions: 40±1℃, 30 days, constant temperature and dark;

[0134] Cold resistance test conditions: -18±2℃, 30 days, constant temperature and away from light;

[0135] Centrifugal test: After centrifugation at 2000 r / min for 30 min, observe whether the sunscreen composition is stratified.

[0136] In the above test, if the sunscreen composition has no stratification, solid precipitation or other system inhomogeneity, the stability test is passed, otherwise the stability test is failed. The results are recorded in Table 4.

[0137] Table 4

[0138] Passed Application Example 1 pass Application Example 2 pass Application Example 3 pass Application Example 4 Not passed Comparative application example 1 pass Comparative Application Example 2 pass Comparative Application Example 3 pass Comparative Application Example 4 pass Comparative Application Example 5 pass Comparative Application Example 6 pass

[0139] From the results in Table 4, it can be seen that the obtained product has good stability. Although the homogenization method in the preparation process of titanium dioxide will not have a great impact on the efficacy of the product, it has a greater impact on the stability of the product. Sunscreen products made from titanium dioxide homogenized by other methods cannot pass the product stability test.

[0140] Test Example 5

[0141] Irritation test

[0142] The samples prepared in Application Examples 1-4 were subjected to patch tests to detect their potential to cause adverse reactions to human skin.

[0143] 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.

[0144] Table 5

[0145] 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

[0146] Table 6

[0147] 1 2 3 4 5 6 Application Example 1 0 0 0 0 0 0 Application Example 2 0 0 0 0 0 0 Application Example 3 0 0 0 0 0 0 Application Example 4 0 0 0 0 0 0

[0148] It can be seen from the data in Table 6 that the sunscreen product prepared from the obtained titanium dioxide is non-irritating and will not cause allergic reactions.

[0149] The applicant declares that the present invention illustrates the preparation method of an active titanium dioxide powder and its product and application through the above-mentioned embodiments, 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 various 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.

[0150] 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.

[0151] 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 active titanium dioxide, characterized in that: The preparation method comprises: (1) mixing Cistanche deserticola with water and performing ultrasonic extraction to obtain an extract; (2) inoculating Lactobacillus rhamnosus and Lactobacillus plantarum into the sterilized extract, and fermenting to obtain a first fermentation product; (3) inoculating the capsule-coated yeast into the first fermentation product, fermenting, and obtaining a second fermentation product; (4) The second fermentation product is centrifuged, filtered, and the supernatant is mixed with titanium dioxide, homogenized, and freeze-dried to obtain active titanium dioxide.

2. The method for preparing active titanium dioxide according to claim 1, characterized in that: The mass ratio of the Cistanche deserticola to water is 1:(5-10); Preferably, the power of the ultrasound is 450-550W, and the time is 25-45min; Preferably, step (1) further comprises mixing the extract with the nutrient substance and sterilizing; Preferably, the nutrients include glucose and peptone; Preferably, the mass percentage of glucose in the sterilized extract is 0.3-0.6%, and the mass percentage of peptone is 0.7-1.5%.

3. The method for preparing active titanium dioxide according to claim 1 or 2, characterized in that: The viable count of Lactobacillus rhamnosus is 4×10 9 CFU / g-8×10 9 CFU / g, inoculum concentration 3-6%; Preferably, the viable count of the plant lactobacillus is 4×10 9 CFU / g-8×10 9 CFU / g, the inoculation amount is 2-5%.

4. The method for preparing active titanium dioxide according to any one of claims 1 to 3, characterized in that: The fermentation temperature in step (2) is 30-35°C, the fermentation time is 6-10 hours, and the pH is 4.5-9.

5.

5. The method for preparing active titanium dioxide according to any one of claims 1 to 4, characterized in that: The number of viable bacteria of the capsule-coated yeast was 4×10 9 CFU / g-8×10 9 CFU / g, the inoculum size was 4-6%.

6. The method for preparing active titanium dioxide according to any one of claims 1 to 5, characterized in that: The fermentation temperature in step (3) is 28-30°C, the fermentation time is 18-30h, and the pH is 4-8.

7. The method for preparing active titanium dioxide according to any one of claims 1 to 6, characterized in that: In step (4), the centrifugal speed is 3000-5000 rpm and the time is 25-35 min; Preferably, the mass ratio of the supernatant to titanium dioxide is 25:(1-2); Preferably, the homogenization method is high-pressure microfluidization homogenization, and the homogenization pressure is 90-160MPa; Preferably, the particle size of the active titanium dioxide is 50-120 nm.

8. An active titanium dioxide prepared by the method for preparing active titanium dioxide according to any one of claims 1 to 7.

9. Use of the active titanium dioxide according to claim 8 in the preparation of sunscreen products.

10. The use according to claim 9, characterized in that: The mass percentage of active titanium dioxide in the sunscreen product is 10-20%.

Images