A sunscreen composition based on the ultraviolet absorption characteristics of Chinese liquor yellow water, and a preparation method and application thereof

Abstract

The application discloses a sunscreen composition based on the ultraviolet absorption characteristics of yellow water of liquor, and a preparation method and application thereof. The sunscreen composition comprises 10-60 parts by weight of a yellow water extract of a strong-flavor liquor, 20-70 parts by weight of a yellow water extract of a Maotai-flavor liquor, and 0-40 parts by weight of a yellow water extract of a light-flavor liquor. It is found that the yellow water of different flavor liquors has characteristic ultraviolet absorption spectrum, wherein the yellow water of the strong-flavor liquor has strong absorption in the UVB band (290-320 nm), the yellow water of the Maotai-flavor liquor has strong absorption in the UVA band (340-380 nm), and the yellow water of the light-flavor liquor has relatively uniform absorption in a wide band. According to the spectral complementarity, the natural sunscreen composition is obtained. The sunscreen composition has an in-vitro SPF value of 15-35, a PA value of ++~++++, good light stability and low skin irritation.

Description

Technical Field

[0001] This invention belongs to the field of sunscreen composition preparation technology, and relates to the fields of cosmetic technology and resource utilization of brewing by-products. Specifically, it is a sunscreen composition based on the ultraviolet absorption characteristics of the yellow water of Baijiu (Chinese liquor), its preparation method and application. Background Technology

[0002] Ultraviolet (UV) radiation is one of the main environmental factors causing sunburn, photoaging, pigmentation, and skin cancer. Based on wavelength, UV radiation is divided into UVA (320-400nm), UVB (280-320nm), and UVC (100-280nm). UVA has strong penetrating power, reaching deep into the dermis and causing photoaging; UVB mainly affects the epidermis, causing sunburn and erythema. Currently, commercially available sunscreens are mainly divided into chemical sunscreens (such as avobenzone and octocrylene) and physical sunscreens (such as titanium dioxide and zinc oxide). While chemical sunscreens offer good sun protection, some ingredients have poor photostability, pose risks of skin irritation, and potential endocrine disruption. Physical sunscreens, while generally safe, tend to leave a white cast and feel heavy on the skin. Naturally derived sunscreen ingredients are gaining increasing attention due to their high safety and environmental friendliness, such as flavonoids, polyphenols, and carotenoids extracted from plants. However, plant extraction is costly, raw material supply is limited by season and region, and the extraction process often requires the use of organic solvents, which does not conform to the concept of green environmental protection.

[0003] Baijiu is a traditional Chinese distilled spirit. During its solid-state fermentation process, a large amount of byproduct—yellow liquid—is produced. This yellow liquid seeps from the bottom of the fermentation pits and is rich in complex components such as organic acids, esters, alcohols, amino acids, phenolic substances, and Maillard reaction intermediates. The brewing processes and microbial communities of different baijiu types (such as strong-aroma, sauce-aroma, and light-aroma baijiu) differ, resulting in significant differences in the chemical composition and physicochemical properties of their yellow liquid.

[0004] In existing technologies, wastewater is mainly used for preparing flavored wines, extracting ethyl hexanoate, or producing organic fertilizers. However, the development of downstream products and treatment processes for wastewater are underdeveloped, resulting in large quantities of wastewater that cannot be treated and reused in a timely manner. Direct discharge of untreated wastewater not only wastes resources but also threatens the environment. Therefore, exploring the development of new products using wastewater to further enhance its utilization value is of great significance. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of existing technologies and provide a sunscreen composition based on the ultraviolet absorption characteristics of the yellow water of baijiu (Chinese white liquor) and its preparation method. Through systematic research, the inventors of this application discovered that the yellow water of different aroma types of baijiu exhibits characteristic absorption peaks in the ultraviolet region, and their absorption spectra are complementary: strong-aroma yellow water shows strong absorption in the UVB band (290-320nm), sauce-aroma yellow water shows strong absorption in the UVA band (340-380nm), while light-aroma yellow water exhibits relatively uniform absorption over a wide wavelength range. Therefore, utilizing this characteristic, the inventors can achieve full-band ultraviolet protection by compounding extracts or treatment solutions of yellow water from different aroma types and applying them for ultraviolet protection. Furthermore, these characteristics can be used to prepare sunscreen products.

[0006] To achieve the above-mentioned objectives, the specific technical solution of this invention is as follows: This invention first protects a sunscreen composition based on the ultraviolet absorption properties of the yellow liquid of baijiu (Chinese white liquor), the sunscreen composition comprising the following components in parts by weight: 10-60 parts by weight of a strong-smelling yellow water extract; 20-70 parts by weight of soy sauce-flavored yellow water extract; 0-40 parts by weight of light-scented yellow water extract.

[0007] As a preferred embodiment of this application, a sunscreen composition based on the ultraviolet absorption properties of the yellow water of baijiu (Chinese white liquor) comprises the following components in parts by weight: 30-50 parts of a strong-smelling yellow water extract; 30-50 parts of soy sauce-flavored yellow water extract 10-20 parts of light-scented yellow water extract.

[0008] In a preferred embodiment of this application, the total phenol content in the sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water is not less than 5 g / L; the total flavonoid content is not less than 2 g / L; and the Maillard reaction intermediate, calculated as 5-hydroxymethylfurfural, has a content of 0.5-3 g / L.

[0009] This invention also protects a method for preparing a sunscreen composition based on the ultraviolet absorption properties of the yellow water of baijiu (Chinese liquor), comprising the following steps: Step 1: Collection and grading of yellow liquids with different aromas The yellow water produced during the solid-state fermentation of strong-aroma, sauce-aroma, and light-aroma baijiu was collected separately, and then filtered through a sieve to remove suspended solids, resulting in coarsely filtered yellow water. The obtained coarsely filtered yellow water was centrifuged, and the supernatant was collected and labeled as strong-aroma yellow water stock solution, soy sauce-aroma yellow water stock solution and light-aroma yellow water stock solution, respectively. In a preferred embodiment of this application, in step one of the preparation method of a sunscreen composition based on the ultraviolet absorption characteristics of baijiu yellow water, the pore size of the sieve for removing solid suspended matter is 60-200 mesh; the centrifugation conditions for coarsely filtering the yellow water are centrifugation at 3000-10000 r / min for 10-30 min.

[0010] Step 2: Ultraviolet absorption spectroscopy analysis and characteristic band calibration The absorption spectra of strong-aroma, soy sauce-aroma, and light-aroma yellow liquors within a specified range were measured using a UV-Vis spectrophotometer. The maximum absorption wavelength λ_max and the corresponding absorbance were recorded, and the average absorbance in the UVA and UVB bands were calculated. Based on the spectral data, the dominant protective bands for each type of yellow liquor were determined: strong-aroma yellow liquor has dominant UVB protection, soy sauce-aroma yellow liquor has dominant UVA protection, and light-aroma yellow liquor is used as a broad-spectrum reinforcing component. In a preferred embodiment of this application, in step two, the absorption spectra of the strong-aroma yellow liquid, the soy sauce-aroma yellow liquid, and the light-aroma yellow liquid are measured in the range of 200-500 nm using a UV-Vis spectrophotometer.

[0011] The optimal ratio of the absorbance of the strong-aroma yellow liquor at 305 nm to that of the soy sauce-aroma yellow liquor at 360 nm is 0.8-1.2. That is, when the ratio of the absorbance of the strong-aroma yellow liquor at 305 nm to that of the soy sauce-aroma yellow liquor at 360 nm is 0.8-1.2, the combination of the two achieves the best spectral balance. The absorption characteristics can also be controlled by adjusting the fermentation cycle or the yellow liquor collection time.

[0012] Step 3: Preparation of Yellow Water Extract The strong-aroma yellow liquid, soy sauce-aroma yellow liquid, and light-aroma yellow liquid obtained in step one are processed sequentially as follows: (1) Microfiltration clarification: Microfiltration is performed using a ceramic membrane or a polyethersulfone membrane to remove bacteria and fine particles, and microfiltrate is obtained; As a preferred embodiment of this application, in step three (1) of the preparation method of a sunscreen composition based on the ultraviolet absorption characteristics of white wine yellow water, microfiltration is performed using a 0.45-1.0μm ceramic membrane or polyethersulfone membrane, the microfiltration operating pressure is 0.1-0.3MPa, and the operating temperature is 25-40℃. (2) Ultrafiltration fractionation: The microfiltrate is fractionated using an ultrafiltration membrane, the permeate is collected, and large molecular proteins and polysaccharides are removed to obtain the ultrafiltrate; As a preferred embodiment of this application, in step (2) of the preparation method of a sunscreen composition based on the ultraviolet absorption characteristics of white wine yellow water, an ultrafiltration membrane with a molecular weight cutoff of 1000-5000 Da is used for grading.

[0013] (3) Vacuum concentration: The ultrafiltrate is concentrated under vacuum to obtain strong aroma yellow water extract (also known as strong aroma yellow water concentrate), soy sauce aroma yellow water extract (also known as soy sauce aroma yellow water concentrate) and light aroma yellow water extract (also known as light aroma yellow water concentrate).

[0014] As a preferred embodiment of this application, in step (3) of the preparation method of a sunscreen composition based on the ultraviolet absorption characteristics of baijiu yellow water, the ultrafiltrate is concentrated to 1 / 10-1 / 5 of its original volume at 50-65℃ and a vacuum degree of 0.08-0.095MPa to obtain strong aroma yellow water extract, soy sauce aroma yellow water extract and light aroma yellow water extract respectively; the total solids content of strong aroma yellow water extract, soy sauce aroma yellow water extract and light aroma yellow water extract is 5wt%-15wt%.

[0015] Step 4: Formulation of sunscreen compositions Weigh out the strong-scented yellow water extract, the soy sauce-scented yellow water extract, and the light-scented yellow water extract according to the specified ratio, then mix and stir them to fully blend them, thus obtaining a liquid sunscreen composition, namely the sunscreen composition stock solution.

[0016] In a preferred embodiment of this application, in step three of the preparation method of a sunscreen composition based on the ultraviolet absorption characteristics of white wine yellow water, the stirring conditions are as follows: stirring at a rate of 100-500 r / min for 15-30 min at 20-40℃.

[0017] As a preferred embodiment of the present invention, in step three, an enzymatic hydrolysis-assisted treatment is added before ultrafiltration fractionation: 0.01%-0.05% of a compound enzyme (cellulase and pectinase, mass ratio 1:1) is added to the microfiltrate of the strong-aroma, soy sauce-aroma, and light-aroma types, respectively, and the mixture is enzymatically hydrolyzed at 40-50℃ for 1-2 hours to release bound phenolic substances and improve the extraction rate of UV-absorbing active ingredients. After enzymatic hydrolysis, the temperature is raised to 85-90℃ for 10 minutes to inactivate the enzyme.

[0018] As a preferred embodiment of the present invention, in step three, a decolorization treatment is added after vacuum concentration: for extracts (liquids) with excessively dark color that affects skin feel, activated carbon (addition amount 0.1%-0.5%) can be used for adsorption and decolorization at 40-50℃ for 15-30 minutes, followed by filtration to remove the activated carbon. This step, while retaining UV absorption activity, changes the color of the extract from dark brown to light yellow, improving the color and skin feel of sunscreen products.

[0019] As a preferred embodiment of the present invention, the sunscreen composition may further contain 0.1%-2% of a physical sunscreen agent (nano titanium dioxide or zinc oxide) to synergistically enhance the sunscreen effect and improve the stability of the formulation.

[0020] As a preferred embodiment of the present invention, the sunscreen composition is subjected to photostability testing before being prepared into a final product: the compounded composition stock solution is placed under an ultraviolet lamp (UVA+UVB, total irradiance 50W / m²) for 2 hours, and the change rate of UVA / UVB absorbance before and after irradiation is measured. A change rate ≤10% is considered qualified.

[0021] This invention also protects the use of the sunscreen composition described in any one of the above claims or the sunscreen composition prepared according to any one of the above claims in full-spectrum ultraviolet protection products or sunscreen products.

[0022] This invention also protects a sun protection product containing a sun protection composition as described in any one of the above claims or a sun protection composition prepared according to the method described.

[0023] As a preferred embodiment of this application, the amount of sunscreen composition added in the sunscreen product is 5wt%-25wt%.

[0024] As a preferred embodiment of this application, the types of sun protection products include sunscreen, sunscreen lotion, sunscreen spray, sunscreen stick, or sunscreen gel, etc.

[0025] As a preferred embodiment of this application, the sunscreen product described above also contains other conventional components that can be prepared as a sunscreen product.

[0026] For example, it can be made according to the following ingredient ratios (in 100% by mass): Sunscreen composition (liquid): 5%-25%; Oily phase (caprylic / capric triglycerides, cetearyl alcohol, etc.): 10%-25%; Emulsifiers (glyceryl stearate, cetearyl alcohol polyether-20, etc.): 3%-8%; Thickeners (xanthan gum, carbomer, etc.): 0.1%-1%; Moisturizers (glycerin, butylene glycol, etc.): 5%-15%; Preservatives (phenoxyethanol, p-hydroxyacetophenone, etc.): 0.5%-1.5%; Deionized water: Balance.

[0027] The preparation method can also employ conventional processes, such as: Heat the aqueous phase components (deionized water, humectant, thickener) to 70-80℃, and heat the oil phase components (oil phase, emulsifier) ​​to 70-80℃. Slowly add the oil phase to the aqueous phase while stirring, and homogenize and emulsify for 3-10 minutes. Cool to below 40℃, add the sunscreen composition and preservative, and stir evenly to obtain the final product.

[0028] The working principle of this invention is as follows: The absorption spectra of each aroma type of yellow liquid (the strong aroma, soy sauce aroma, and light aroma yellow liquid obtained in step one) in the range of 200-500 nm were measured using a UV-Vis spectrophotometer. The maximum absorption wavelength λ_max and the corresponding absorbance were recorded, and the average absorbance of each band (UVA, UVB) was calculated. Based on the spectral data, the dominant protective bands of each aroma type of yellow liquid were determined: the strong aroma type of yellow liquid has dominant UVB protection, the soy sauce aroma type of yellow liquid has dominant UVA protection, and the light aroma type of yellow liquid is used as a broad-spectrum reinforcing component.

[0029] Measurements showed that the yellow aqueous extract of strong-aroma baijiu exhibited a maximum absorption peak (strong absorption) in the 290-320 nm wavelength range, with a peak absorbance ≥1.5 (1% dilution, 1 cm cuvette); the yellow aqueous extract of sauce-aroma baijiu exhibited a maximum absorption peak (strong absorption) in the 340-380 nm wavelength range, with a peak absorbance ≥1.2 (1% dilution, 1 cm cuvette); and the yellow aqueous extract of light-aroma baijiu exhibited an absorbance ≥0.8 (1% dilution, 1 cm cuvette) in the 280-400 nm range, indicating that the light-aroma yellow aqueous extract showed relatively uniform absorption over a wide wavelength range. The yellow aqueous extracts of different baijiu types all exhibited characteristic absorption peaks in the ultraviolet region, and their absorption spectra showed complementarity.

[0030] Compared with existing technologies, the beneficial effects of this invention are: (1) This invention is the first to apply the yellow water, a byproduct of baijiu brewing, to the field of sun protection, realizing the high-value resource utilization of waste. This invention uses the yellow water generated in large quantities during the production of strong-aroma, sauce-aroma, and light-aroma baijiu as raw material, turning waste into treasure. Every ton of baijiu produced can generate 3-5 tons of yellow water, which would cause serious environmental pollution if directly discharged. This invention provides a brand-new high-value-added application path for yellow water, with both environmental and economic benefits.

[0031] (2) This invention utilizes the complementarity of the ultraviolet absorption spectra of different aroma types of yellow water to achieve broad-spectrum and highly efficient ultraviolet protection. This invention is the first to systematically study the ultraviolet absorption characteristics of different aroma types of yellow water, and found that the strong aroma type yellow water is rich in phenolic acid components (such as ferulic acid and p-coumaric acid), and has strong absorption in the UVB band; the soy sauce aroma type yellow water produces more melanoidins and polypyrroles due to the high-temperature stacking process, and has prominent absorption in the UVA band; the light aroma type yellow water has relatively simple components but a broad absorption spectrum. Through scientific compounding, full-band coverage can be achieved, with an in vitro SPF value of 15-35 and a PA value of ++++.

[0032] (3) The preparation method in this invention is green and environmentally friendly, does not use organic solvents, and conforms to the "pure beauty" trend in the cosmetics industry. This invention uses physical methods such as aqueous phase extraction, membrane separation and vacuum concentration, does not use organic solvents throughout the process, has no harmful residues, and conforms to the concepts of green chemistry and sustainable manufacturing.

[0033] (4) The raw materials in this invention are naturally sourced, highly safe, and possess both antioxidant and anti-inflammatory activities. The phenolic and flavonoid components in the yellow water, in addition to absorbing ultraviolet rays, also have additional effects such as scavenging free radicals and inhibiting tyrosinase, and can be used to develop multifunctional products that combine sun protection, whitening, and anti-aging. Patch testing has verified that the sun protection composition of this invention is non-irritating to the skin and has good safety.

[0034] (5) The raw materials used in this invention are widely available, inexpensive, and simple to process, making them easy to industrialize. Yellow water is a "waste" of liquor enterprises, and the cost of obtaining the raw materials is extremely low. The process flow of this invention is short, the equipment requirements are conventional, and it is easy to establish a supporting cosmetic raw material production line in liquor production areas.

[0035] (6) The preservatives (phenoxyethanol and p-hydroxyacetophenone) used in this invention meet the requirements of the "Cosmetic Safety Technical Specifications", and the concentrations used are all within the national allowable range, ensuring product safety. Attached Figure Description

[0036] Figure 1 The UV-Vis absorption spectra (200-500nm) of the raw yellow liquid of strong-aroma (baijiu), sauce-aroma (baijiu), and light-aroma (baijiu) are shown.

[0037] Figure 2 This is a comparison of the ultraviolet absorption spectra of sunscreen compositions with different compounding ratios.

[0038] Figure 3 The photostability comparison curves of the sunscreen composition stock solution prepared in Example 1 of the present invention and commercially available chemical sunscreens (avobenzone + octocrylene) are shown.

[0039] Figure 4The bar chart shows the in vitro SPF value determination results of the sunscreen prepared in Example 7 of this invention and the blank matrix.

[0040] Figure 5 The graph shows the correlation between the total phenol content and ultraviolet absorbance of yellow water extracts with different aroma types.

[0041] Figure 6 A comparison chart showing the content of major phenolic acids in yellow water with different aromas.

[0042] Figure 7 A comparison chart showing the SPF values ​​and photostability of sunscreen compositions with different compounding ratios. Detailed Implementation

[0043] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0044] It should be noted that the following detailed descriptions are illustrative and intended to provide further explanation of this application. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains.

[0045] It should be noted that the terminology used herein is for the purpose of describing particular implementations only and is not intended to limit the exemplary implementations according to this application. As used herein, the singular form includes the plural form unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this description, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0046] In this invention, some conventional operating equipment, devices and components have been omitted or only briefly described.

[0047] Unless otherwise specified in the examples, the conditions shall be performed according to the standard conditions or the conditions recommended by the manufacturer.

[0048] In this application, any percentage not marked indicates its weight percentage content.

[0049] Example 1 A sunscreen composition based on the ultraviolet absorption properties of the yellow liquid of Baijiu (Chinese white liquor), the preparation method of which includes the following steps: Step 1: Collection and grading of yellow liquids with different aromas 100L of yellow liquid discharged during the normal fermentation cycles of three liquor enterprises in Sichuan Province were collected (i.e., 100L of yellow liquid produced during the solid-state fermentation of strong-aroma liquor, 100L of yellow liquid produced during the solid-state fermentation of sauce-aroma liquor, and 100L of yellow liquid produced during the solid-state fermentation of light-aroma liquor). Each yellow liquid was filtered through a 100-mesh sieve to remove solid residues such as sorghum husks and wheat bran. Then, it was centrifuged at 6000 rpm for 15 minutes, and the supernatant was collected to obtain the original yellow liquid solutions for strong-aroma, sauce-aroma, and light-aroma liquors, respectively.

[0050] Step 2: Ultraviolet absorption spectroscopy analysis and characteristic band calibration The absorption spectra of three yellow water stock solutions in the 200-500 nm range were measured using a Shimadzu UV-2600 UV-Vis spectrophotometer, with deionized water as a reference, in a 1 cm quartz cuvette. The results are as follows: Strongly aromatic yellow liquid concentrate: The maximum absorption peak is located at 305nm, and the absorbance is 1.68 (1% dilution); the average absorbance in the UVB band (280-320nm) is 1.52; and the average absorbance in the UVA band (320-400nm) is 0.63.

[0051] Soy sauce flavored yellow liquid: The maximum absorption peak is located at 365nm, and the absorbance is 1.42 (1% dilution); the average absorbance in the UVA band is 1.28; and the average absorbance in the UVB band is 0.71.

[0052] Lightly scented yellow liquid concentrate: The absorption peak is relatively flat, with the maximum absorption at 285nm and an absorbance of 0.92 (1% dilution); the average absorbance in the 280-400nm range is 0.81.

[0053] For details, please see [link / details]. Figure 1 , Figure 1 The UV-Vis absorption spectra (200-500 nm) of the raw yellow liquid from strong-aroma, sauce-aroma, and light-aroma baijiu are shown. Figure 1 It can be seen that the strong aroma type yellow liquor has a strong absorption peak at 305nm, the soy sauce aroma type yellow liquor has a strong absorption peak at 365nm, and the light aroma type yellow liquor has relatively uniform absorption in the range of 280–400nm.

[0054] Step 3: Preparation of Yellow Water Extract Take 50L of each type of yellow liquid concentrate and process them as follows: (1) Microfiltration clarification: A 0.45μm ceramic membrane was used, the operating pressure was 0.2MPa, the temperature was 30℃, and about 48L of microfiltrate was collected.

[0055] (2) Ultrafiltration fractionation: The microfiltrate was filtered using a polyethersulfone ultrafiltration membrane with a molecular weight cutoff of 3000 Da, the operating pressure was 0.3 MPa, and about 42 L of permeate was collected.

[0056] (3) Vacuum concentration: The ultrafiltrate was concentrated to 1 / 8 of its original volume at 60℃ and a vacuum of 0.09MPa to obtain approximately 5.2L of concentrated extracts of each aroma type. Analysis showed that the total phenol content in the strong aroma type extract was 7.8g / L, and the total flavonoid content was 3.2g / L; the total phenol content in the soy sauce aroma type extract was 6.5g / L, the total flavonoid content was 2.5g / L, and the 5-hydroxymethylfurfural content was 2.1g / L; and the total phenol content in the light aroma type extract was 4.2g / L, and the total flavonoid content was 1.6g / L.

[0057] Step 4: Formulation of sunscreen compositions Based on the spectral data from step two, the following components by weight were compounded: 40 parts of a strong-scented yellow water extract, 40 parts of a soy sauce-scented yellow water extract, and 20 parts of a light-scented yellow water extract. The yellow water extracts were directly mixed and stirred at 300 rpm for 20 minutes at 30°C to obtain the sunscreen composition (also known as the sunscreen composition stock solution).

[0058] Tests: In vitro SPF value determination (according to ISO 24443:2012 standard, using a Labsphere UV-2000S ultraviolet transmittance analyzer): SPF value 28.6, PA value +++. Photostability test: After 2 hours of ultraviolet irradiation, the SPF value remained at 26.4, with a decrease rate of 7.7%.

[0059] Example 2 A sunscreen composition based on the ultraviolet absorption properties of the yellow water of baijiu (Chinese white liquor) is prepared using a method essentially the same as in Example 1, except that the compounding ratio of the various aroma types of yellow water extracts in step four is different. Specifically, by weight, the composition contains 50 parts of the strong aroma type yellow water extract, 30 parts of the soy sauce aroma type yellow water extract, and 20 parts of the light aroma type yellow water extract.

[0060] The prepared sunscreen composition (stock solution) was tested and found to have an SPF of 22.4 and a PA rating of ++. This formulation prioritizes UVB protection and is suitable for daily commutes.

[0061] Example 3 A sunscreen composition based on the ultraviolet absorption characteristics of the yellow water of Baijiu (Chinese liquor) is prepared in a manner that is basically the same as in Example 1, except that an enzymatic hydrolysis auxiliary treatment is added in step three: before ultrafiltration fractionation, 0.03% of a compound enzyme (the mass ratio of cellulase to pectinase is 1:1) is added to the supernatant of each type of yellow water, and the mixture is hydrolyzed at 45°C for 1.5 h, and then the temperature is raised to 90°C to inactivate the enzyme for 10 min.

[0062] According to the test results, after this treatment, the total phenol content of the strong-scented yellow water extract increased from 7.8 g / L to 10.2 g / L, the ultraviolet absorbance increased by about 28%, and the SPF value of the prepared sunscreen composition stock solution increased from 28.6 to 34.2.

[0063] Example 4 A sunscreen composition based on the ultraviolet absorption properties of the yellow water of baijiu (Chinese white liquor) is prepared using a method essentially the same as in Example 1, except that the compounding ratio of the sunscreen composition differs in step four. Specifically, by weight, the composition comprises 30 parts of a strong-aroma type of yellow water extract, 50 parts of a soy sauce-aroma type of yellow water extract, and 20 parts of a light-aroma type of yellow water extract.

[0064] The prepared sunscreen composition (stock solution) was tested and found to have an SPF of 26.1 and a PA rating of ++++. This formulation places greater emphasis on UVA protection, making it suitable for outdoor activities or scenarios requiring high levels of protection against photoaging.

[0065] Example 5 A sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water is prepared in a manner that is basically the same as in Example 1, except that in step four, after the sunscreen composition is compounded, a step of synergistic effect with physical sunscreen agents is added: the sunscreen composition (stock solution) obtained in Example 1 is mixed with nano titanium dioxide at a weight ratio (stock solution: nano titanium dioxide = 10:1), that is, 1% by mass of nano titanium dioxide is added based on the mass of the sunscreen composition stock solution, and the mixture is stirred at 400 r / min for 30 min at 40°C to obtain a synergistic sunscreen composition with compounded physical sunscreen agents.

[0066] Tests showed that the resulting synergistic sunscreen composition had an SPF of 35.2 and a PA rating of ++++, providing more balanced UVA / UVB protection and a refreshing feel without leaving a white cast.

[0067] Example 6 This embodiment provides a sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water, suitable for industrial production. Its preparation method is basically the same as in Example 1, with the only difference being the process parameters of each step: Step 1: Use an industrial-grade disc centrifuge (7200 r / min, 500 L / h flow rate) instead of a laboratory centrifuge for continuous separation.

[0068] Step 2: The ultraviolet absorption spectroscopy analysis was replaced with an online detection system (Systag FlexAct®) to achieve real-time monitoring and data feedback of the absorption characteristics of each type of yellow liquid.

[0069] Step 3: The membrane separation system is upgraded to industrial-grade equipment, in which microfiltration uses a 0.5μm ceramic membrane (operating pressure 0.25MPa, temperature 35℃), ultrafiltration uses a spiral wound organic membrane with a molecular weight cutoff of 2000Da (operating pressure 0.35MPa), and vacuum concentration uses a triple-effect evaporator (60℃, vacuum degree 0.09MPa) to concentrate to 1 / 8 of the original volume.

[0070] Step 4: The compounding process uses an automatic batching system to continuously mix 40 parts of strong-scented yellow water extract, 40 parts of soy sauce-scented yellow water extract, and 20 parts of light-scented yellow water extract. The mixture is fully blended at 30°C using a static mixer to obtain the sunscreen composition (stock solution).

[0071] The SPF value was 29.1 and the PA value was +++.

[0072] Each step in this embodiment uses industrial-grade equipment, realizing the transformation from laboratory scale to industrial production. The process is stable and controllable, and the produced sunscreen composition concentrate has uniform quality, making it suitable for establishing a supporting cosmetic raw material production line in liquor-producing areas.

[0073] Example 7 A sunscreen, formulated according to the following weight percentages (total 100g): The sunscreen composition stock solution prepared in Example 1: 15g; Caprylic / capric triglyceride: 8g; Cetearyl alcohol: 4g; Glyceryl stearate: 3g; Cetearyl alcohol polyether-20: 2g; Xanthan gum: 0.2g; Glycerin: 5g; 1,3-Butanediol: 3g; Phenoxyethanol: 0.8g; Deionized water: Add to 100g.

[0074] Preparation method: Deionized water, glycerin, 1,3-butanediol, and xanthan gum were mixed and heated to 75°C to form the aqueous phase; caprylic / capric triglyceride, cetearyl alcohol, glyceryl stearate, and cetearyl alcohol polyether-20 were mixed and heated to 75°C to form the oil phase; the oil phase was slowly added to the aqueous phase under stirring and homogenized and emulsified for 5 minutes; the mixture was cooled to below 40°C, and the sunscreen composition stock solution prepared in Example 1 and phenoxyethanol were added and stirred evenly to obtain the sunscreen.

[0075] The resulting sunscreen is a light yellow cream with a fine texture that is easy to apply.

[0076] A patch test was conducted on the backs of 10 volunteers (aged 22-45, 5 men and 5 women). No irritation reactions such as erythema or edema were observed after 48 hours. Tests: Human SPF values ​​were determined (in vivo method modified according to the 2015 edition of the "Cosmetic Safety Technical Specifications"): the average SPF value was 25.3, and the PFA value was 8.2 (equivalent to PA+++).

[0077] Comparative Example 1 A sunscreen composition was prepared using a single-fragrance yellow water extract (100 parts by weight of strong-fragrance yellow water extract only), and the remaining methods and steps were the same as in Example 1.

[0078] The tested sunscreen material had an SPF of 15.3, but insufficient UVA protection, a PA value of only +, and an SPF of 9.8 after 2 hours of UV exposure (a decrease of 36%). Its photostability was significantly worse than that of the compound product in Example 1.

[0079] Comparative Example 2 Commercially available chemical sunscreen (3% avobenzone + 5% octocrylene) was used as the active ingredient, and the other excipients were the same as in Example 7 to prepare the sunscreen (the preparation of the sunscreen was the same as in Example 7, except that 15g of the sunscreen composition stock solution prepared in Example 1 was replaced with 15g of the commercially available chemical sunscreen; all other methods and steps were the same).

[0080] In vitro SPF testing showed that the sunscreen initially had an SPF of 32.5 and a PA rating of +++. After 2 hours of UV exposure, the SPF dropped to 18.2, a decrease of 44.0%, indicating significantly inferior photostability compared to the compound product of this invention (which showed a decrease of only 7.7% in Example 7). Furthermore, patch tests showed that two volunteers experienced mild erythema reactions to the commercially available sunscreen, while the product of this invention showed no irritation.

[0081] Comparative Example 3 Baicalin was extracted from Scutellaria baicalensis using a water extraction and alcohol precipitation method as a natural sunscreen agent (refer to method CN 104887544 A). Sunscreen was prepared with the same amount of active ingredient added (the total solids content in the natural sunscreen agent was equivalent to the total solids content in the sunscreen composition obtained in Example 1). The preparation of the sunscreen was the same as in Example 7, except that 15g of the sunscreen composition stock solution prepared in Example 1 was replaced with 15g of the natural sunscreen agent.

[0082] Testing revealed that the total phenolic content of the baicalin extract was 9.5 g / L, with baicalin (a flavonoid) as the main component. Its maximum UV absorption was located at 276 nm, exhibiting strong absorption in the UVB band (peak absorbance 1.42) but weak absorption in the UVA band (peak absorbance 0.35), indicating incomplete spectral coverage. The resulting sunscreen had an in vitro SPF of 18.6 and a PA rating of +. After 2 hours of UV irradiation, the SPF dropped to 15.3 (a decrease of 17.7%). Furthermore, this extraction process requires ethanol as a solvent, which does not meet environmental protection requirements, and the raw material cost is 15 times that of Example 1, making it less economical.

[0083] test: 1. The sunscreen compositions obtained in Examples 1, 2, and 4 were compared with the UV absorption spectra of a single-fragrance yellow water extract. See details below. Figure 2 , Figure 2 This is a comparison of the UV absorption spectra of sunscreen compositions with different formulation ratios. Figure 2 It can be seen that with the increase of the proportion of strong-aroma yellow water extract, the absorption of UVB band (290–320nm) is significantly enhanced; with the increase of the proportion of soy sauce-aroma yellow water extract, the absorption of UVA band (340–380nm) is significantly improved; the addition of light-aroma yellow water extract helps to fill the absorption valley and achieve uniform absorption across a wide band.

[0084] 2. The photostability of the sunscreen composition obtained in Example 1 was compared with that of commercially available chemical sunscreens. See the attached table for details. Figure 3 ; Figure 3 The photostability comparison curves of the sunscreen composition stock solution prepared in Example 1 of this invention and commercially available chemical sunscreens (avobenzone + octocrylene) are shown. Figure 3 It can be seen that after 2 hours of ultraviolet irradiation, the SPF value of the sunscreen composition of the present invention decreased by only 7.7%, while the SPF value of commercially available chemical sunscreens decreased by as much as 44.0%, indicating that the composition of the present invention has better photostability.

[0085] 3. The sunscreen prepared in Example 7 of this invention and a blank matrix (referring to a basic formula without any added sunscreen active ingredients, i.e., without the sunscreen composition described in this invention, with all other substances being the same) were subjected to in vitro SPF value determination. The columnar results are shown in the figure. Figure 4 .from Figure 4 It can be seen that the SPF value of the sunscreen containing the sunscreen composition of the present invention is significantly higher than that of the blank matrix, indicating that the composition has good ultraviolet protection ability.

[0086] 4. Correlation analysis was performed on the total phenolic content and ultraviolet absorbance of the different aroma-type yellow water extracts obtained in Example 1. Specific results are shown in [link to results]. Figure 5 . Figure 5Correlation analysis graph showing the total phenol content and UV absorbance of yellow water extracts with different aroma types. From Figure 5 It can be seen that the total phenol content is positively correlated with the ultraviolet absorbance. The total phenol content of the strong-aroma yellow water extract is the highest, and its ultraviolet absorption is the strongest. The total phenol content of the light-aroma yellow water extract is relatively low, but its ultraviolet absorption spectrum is wider.

[0087] 5. The contents of the main phenolic acids in the different aroma-type yellow water extracts obtained in Example 1 were compared. See the results below for details. Figure 6 . Figure 6 A comparison chart showing the content of major phenolic acids in yellow water extracts of different aroma types. From Figure 6 It can be seen that the strong-aroma yellow water has a high content of ferulic acid and p-coumaric acid, the soy sauce-aroma yellow water is rich in melanin precursor substances, and the light-aroma yellow water has a variety of phenolic acid substances but a low content. The differences in the components of the three constitute the basis for the complementary ultraviolet absorption.

[0088] 6. Different aroma-type yellow water extracts were mixed in different proportions, and their SPF values ​​and photostability were then measured. Specific results are shown in [link to results]. Figure 7 . Figure 7 This is a comparison chart of SPF values ​​and photostability of sunscreen compositions with different formulation ratios. Figure 7 It can be seen that when the compound ratio of strong aroma, soy sauce aroma and light aroma yellow water extract is 40:40:20, the SPF value is the highest and the photostability is the best, indicating that this ratio achieves the optimal balance between UV protection effect and stability.

[0089] The embodiments described above merely illustrate specific implementation methods of this application, and while the descriptions are detailed, they should not be construed as limiting the scope of protection of this application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the technical solution of this application, and these modifications and improvements all fall within the scope of protection of this application.

[0090] This background section is provided to generally present the context of the invention. The work of the currently named inventors, the work to the extent described in this background section, and aspects described in this section that did not constitute prior art at the time of application are neither expressly nor impliedly acknowledged as prior art to the invention.

Claims

1. A sunscreen composition based on the ultraviolet absorption properties of the yellow liquid of Baijiu (Chinese white liquor), characterized in that, The sunscreen composition comprises the following components in parts by weight: 10-60 parts by weight of a strong-smelling yellow water extract; 20-70 parts by weight of soy sauce-flavored yellow water extract; 0-40 parts by weight of light-scented yellow water extract.

2. The sunscreen composition based on the ultraviolet absorption properties of the yellow liquid of Baijiu (Chinese liquor) according to claim 1, characterized in that, The sunscreen composition comprises the following components in parts by weight: 30-50 parts of a strong-smelling yellow water extract; 30-50 parts of soy sauce-flavored yellow water extract 10-20 parts of light-scented yellow water extract.

3. A sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water according to claim 1 or 2, characterized in that: In the sunscreen composition, the total phenol content is not less than 5 g / L; the total flavonoid content is not less than 2 g / L; and the Maillard reaction intermediate, calculated as 5-hydroxymethylfurfural, has a content of 0.5-3 g / L.

4. The method for preparing a sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water according to claim 3, characterized in that... Includes the following steps: Step 1: Collection and grading of yellow liquids with different aromas The yellow water produced during the solid-state fermentation of strong-aroma, sauce-aroma, and light-aroma baijiu was collected separately, and then filtered through a sieve to remove suspended solids, resulting in coarsely filtered yellow water. The obtained coarsely filtered yellow water was centrifuged, and the supernatant was collected and labeled as strong-aroma yellow water stock solution, soy sauce-aroma yellow water stock solution and light-aroma yellow water stock solution, respectively. Step 2: Ultraviolet absorption spectroscopy analysis and characteristic band calibration The absorption spectra of strong-aroma, soy sauce-aroma, and light-aroma yellow liquors within a specified range were measured using a UV-Vis spectrophotometer. The maximum absorption wavelength λ_max and the corresponding absorbance were recorded, and the average absorbance in the UVA and UVB bands were calculated. Based on the spectral data, the dominant protective bands for each type of yellow liquor were determined: strong-aroma yellow liquor has dominant UVB protection, soy sauce-aroma yellow liquor has dominant UVA protection, and light-aroma yellow liquor is used as a broad-spectrum reinforcing component. Step 3: Preparation of Yellow Water Extract The strong-aroma yellow liquid, the soy sauce-aroma yellow liquid, and the light-aroma yellow liquid obtained in step one are respectively processed as follows: (1) Microfiltration clarification: Microfiltration is performed using ceramic membranes or polyethersulfone membranes to remove bacteria and fine particles, resulting in strong-aroma yellow water microfiltrate, soy sauce-aroma yellow water microfiltrate, and light-aroma yellow water microfiltrate, respectively. (2) Ultrafiltration classification: The obtained strong aroma yellow water microfiltrate, soy sauce aroma yellow water microfiltrate and light aroma yellow water microfiltrate are classified by ultrafiltration membrane, the permeate is collected, and large molecular proteins and polysaccharides are removed to obtain strong aroma yellow water ultrafiltrate, soy sauce aroma yellow water ultrafiltrate and light aroma yellow water ultrafiltrate respectively. (3) Vacuum concentration: The strong aroma yellow water ultrafiltrate, the soy sauce aroma yellow water ultrafiltrate and the light aroma yellow water ultrafiltrate were vacuum concentrated to obtain strong aroma yellow water extract, soy sauce aroma yellow water extract and light aroma yellow water extract, respectively. (4) Ultraviolet absorption spectroscopy determination: The absorbance of the yellow water extracts of strong aroma type, soy sauce aroma type and light aroma type in the 280–400 nm band was measured respectively to guide the subsequent compounding ratio. Step 4: Formulation of sunscreen compositions Weigh out the strong-scented yellow water extract, the soy sauce-scented yellow water extract, and the light-scented yellow water extract obtained in step three according to the specified ratio, then mix and stir them to fully blend them, thus obtaining a liquid sunscreen composition.

5. The method for preparing a sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water according to claim 4, characterized in that: In step one, the sieve used to remove suspended solids has a mesh size of 60-200 mesh; the centrifugation conditions for coarsely filtered yellow water are 3000-10000 r / min for 10-30 min; in step two, the absorption spectra of the strong-aroma yellow water stock solution, the soy sauce-aroma yellow water stock solution, and the light-aroma yellow water stock solution in the range of 200-500 nm are measured using a UV-Vis spectrophotometer; the ratio of the absorbance of the strong-aroma yellow water stock solution at 305 nm to the absorbance of the soy sauce-aroma yellow water stock solution at 360 nm is 0.8-1.

2.

6. The method for preparing a sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water according to claim 4, characterized in that: In step three, (1) microfiltration clarification, a 0.45-1.0 μm ceramic membrane or polyethersulfone membrane is used for microfiltration. The operating pressure of microfiltration is 0.1-0.3 MPa, and the operating temperature is 25-40℃; (2) ultrafiltration fractionation, an ultrafiltration membrane with a molecular weight cutoff of 1000-5000 Da is used for fractionation; (3) vacuum concentration, the ultrafiltrate is concentrated to 1 / 10-1 / 5 of its original volume under conditions of 50-65℃ and a vacuum degree of 0.08-0.095 MPa, respectively, to obtain concentrated yellow water extract of strong aroma, concentrated yellow water extract of soy sauce aroma, and concentrated yellow water extract of light aroma; concentrated yellow water extract of strong aroma, concentrated yellow water extract of soy sauce aroma, and concentrated yellow water extract of light aroma The total solids content in the concentrate is 5wt%-15wt%. An enzymatic hydrolysis-assisted treatment step is added before ultrafiltration fractionation, specifically, 0.01wt%-0.05wt% of a compound enzyme (a mixture of cellulase and pectinase in a 1:1 mass ratio) is added to the microfiltrates of the strong-aroma, soy sauce-aroma, and light-aroma types, respectively. The enzyme is then inactivated after hydrolysis at 40-50℃ for 1-2 hours. After vacuum concentration, a decolorization treatment is added, where activated carbon is used to adsorb and decolorize the strong-aroma, soy sauce-aroma, and light-aroma extracts at 40-50℃ for 15-30 minutes, with the activated carbon added at 0.1%-0.5% of the volume of each extract.

7. The method for preparing a sunscreen composition based on the ultraviolet absorption properties of baijiu yellow water according to claim 4, characterized in that: In step four, the stirring conditions are: stirring at 100-500 r / min for 15-30 min at 20-40℃.

8. The use of the sunscreen composition according to any one of claims 1-3 or the sunscreen composition prepared by the method according to any one of claims 4-7 in full-spectrum ultraviolet protection products or sunscreen products.

9. A sunscreen product, characterized in that: The sunscreen composition comprising any one of claims 1-3 or the sunscreen composition prepared by the method according to any one of claims 4-7.

10. The sun protection product according to claim 9, characterized in that: In the sunscreen product, the amount of sunscreen composition added is 5wt%-25wt%.

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