Cosmetic raw material from lily waste, its extraction process and use.

Description

1 / 11 “COSMETIC RAW MATERIAL FROM LILY WASTE, ITS OBTAINING PROCESS AND USE”

[001] This invention patent pertains to the technical field of developing a standardized cosmetic active ingredient in flavonoids, obtained from upcycling the residue of lily parts, more specifically from the species Lilium orientalis Stargazer, which is the approved species used for the extraction of essential oil, as it has the best olfactory properties for use in the Lily fragrance, through the application of a sustainable raw material obtaining process by utilizing all residues composed of stems, petal residue (after essential oil extraction), filaments and anthers, followed by standardization. STATE OF THE ART

[002] There are several raw materials on the market obtained from fresh lily plants, of various species available. For example, the company Aqia Química Inovativa offers a raw material of the species Iris Florentina Root Extract, obtained from the root. In turn, the company Cosmético Livre offers a hydrosol (distilled water and plant) of the species Hedychium coronarium (Swamp Lily).

[003] Among the patent documentation that refers to Lilium Stargazer, the subject of the present invention, document US2015045287 mentions a method of controlling or combating microbial organisms by applying an antimicrobial peptide derived from a protein of Lilium 'Stargazer'.

[004] Among the non-patent literature, the article entitled “Potential Applications of Lilium Plants in Cosmetics: A Comprehensive Review Based on Research Papers and Patents” (Jun Ming et al, 2022), published at https: / / www.mdpi.com / 20763921 / 11 / 8 / 1458, describes that with the improvement of people's living standards, aesthetic demands are increasing, leading to the increasingly extensive use of cosmetics, with consumer goods derived from natural resources being increasingly sought after due to awareness of sustainable production and long-term health benefits. In this sense, it highlights the genus Lilium as a resource from the plant family in cosmetics based on natural products, which includes more than 100 species. Petition 870250066393, dated 07 / 30 / 2025, page 9 / 10 2 / 11 wild varieties and thousands of cultivars, and indicates that phytochemical studies prove that the Lilium plant is rich in bioactive components such as phenolic acids, flavonoids and polysaccharides, important base components for its application in cosmetics. TECHNICAL PROBLEM

[005] Although the state of the art predicts potential qualities of Lilium, with applications ranging from antimicrobial to, more specifically, its application in cosmetics, it does not describe a process for obtaining a product that utilizes all lily residues in specific proportions, especially after the extraction of essential oil from the petals, even more specifically from the Lilium orientalis Stargazer species. This leads to problems regarding the accumulation of residues generated in obtaining lily extracts, since the raw material obtaining processes only use the petals or the root, unlike the process described here, configuring a typical upcycling process.

[006] For example, document US2015045287 is limited to dealing with a study of an antimicrobial peptide agent derived from a protein of Lilium Stargazer. In turn, the document Jun Ming et al (2022) presents an analysis of the potential cosmetic application of lily, a study of various plant parts of different lily species and discusses cosmetic action, however it does not mention a method of obtaining raw material that utilizes all the residues of the lily, specifically Lilium orientalis Stargazer. TECHNICAL SOLUTION

[007] The present invention seeks to solve the problem of waste accumulation generated in the processes of obtaining raw material from lilies known in the state of the art by using all the waste from the lily of the species Lilium orientalis Stargazer, including the petal after extraction of the essential oil (enfleurage), stem, filament and anther, which would usually be discarded.

[008] The raw material of Lilium orientalis Stargazer of the present invention differs from other lily raw materials on the market because it does not originate from the raw material but rather from a residue of previously processed material. Furthermore, the Petition 870250005852, dated 01 / 24 / 2025, p. 13 / 25 3 / 11 The present invention also differs from the state of the art with regard to the method of obtaining the raw material, the use of residue from the entire plant and the proportion of plant parts used, since the raw material currently on the market uses only lily petals or petals associated with their root.

[009] The present invention provides a standardized cosmetic active ingredient rich in flavonoids resulting from an extraction process that uses predefined proportions of plant parts to ensure the highest quantity of functional ingredients (polyphenols / flavonoids) in the final product. This raw material, obtained from all the residues of the lily species Lilium orientalis Stargaze, will be produced on an industrial scale for application in cosmetic products. Among all the methods evaluated – including aqueous extraction, hydroalcoholic extraction, and subcritical water extraction (SbcrW) – the present invention uses hydroalcoholic extraction because it offers the best desired result. This type of extraction, from the mixture of residue parts in defined and previously studied proportions, guarantees the highest quantity of active and functional components (polyphenols / flavonoids), generating a raw material with antioxidant activity.Several proportions were tested and, based on the results obtained, the proportion to be processed was defined as 2 parts petal residue (after essential oil extraction), 2 parts filaments, 0.5 parts anthers, and 0.5 parts stems (stalks). Table 1 below shows the amount of polyphenols and flavonoids in the parts: Table 1. Parts. Concentration of raw material (mg / mL). Polyphenols (mg gallic acid equivalent / g raw material). Total Flavonoids (Lg / mL). Petal residues 4.310 5.970 25.700. Anthers 3.965 3.400 12.350. Filaments 4.370 3.735 16.350. Stems 7.846 1.280 10.000

[0010] Obtaining a raw material in an unusual way according to the present invention comprises a process in which the petals are firstly Petition 870250005852, dated 01 / 24 / 2025, page 14 / 25 4 / 11 are separated and used for the extraction of essential oil, by the enfleurage process, to be used in perfumes. After this process, the residue of these petals is separated for drying. The remaining parts of the plant are separated into parts: stems, pistils and anthers, which are then taken to dry separately. After the drying process, the parts are separately sent to the hydroalcoholic extraction stage. According to the present invention, for this process, water and alcohol are used in a one-to-one ratio (and a predefined quantity of lily parts, with the petals and filaments being in a much larger proportion than the anthers and stems (2:2:0.5:0.5)).

[0011] According to the present invention, advantageously compared to the prior art, all residual material from the lily, which would be discarded after the essential oil extraction process from the petals (used in perfumery), is used to enhance the fragrance in the final olfactory process, resulting in the development of a new raw material to be applied on an industrial scale in skincare products due to its antioxidant properties.

[0012] In an unusual way compared to the state of the art, in addition to using the stems, anthers, filaments and petal residue, since the petals in their natural state previously undergo an essential oil extraction process before being subjected to drying and hydroalcoholic extraction, unique and standardized quantities of each part are used to extract the best and most concentrated functional actives from the plant. This ideal proportion is 2 parts petal residue, 2 parts filaments, 0.5 parts stems and 0.5 parts anthers. The ideal, so-called "optimal" proportion is calculated and achieved based on the polyphenol concentration of each part of the plant.

[0013] This lily raw material was subjected to the ORAC test for determination of antioxidant activity and exhibits superior antioxidant activity to Vitamin C, for example, which is now known worldwide for this purpose, and for this reason the material of this present invention can be applied in product lines for skin care.

[0014] Since the ORAC method is the antioxidant activity test performed, as Petition 870250005852, dated 01 / 24 / 2025, page 15 / 25 The 5 / 11 standard for this activity was Trolox, which has a high antioxidant activity. The sample evaluated showed a result of 160.5 Trolox equivalents. This means that 1 mL of the object of the present invention has an antioxidant action equivalent to 160.5 mM of Trolox, which in turn is equivalent to 53.71 g of vitamin C (compared to literature data).

[0015] The raw material was also subjected to in vitro efficacy tests and the following benefits can be highlighted: • It plays a role in processes involved in cell regeneration and renewal; • Cellular detoxification; • Antioxidant action; • Protection against oxidative stress; • Protection against free radicals and pollutants; • Contributes to the integrity of the skin barrier; • Prevention of water loss; • It acts by increasing the expression of several genes responsible for the production of multiple collagens in the skin by between 56% and 99%.

[0016] Therefore, with the use of the tested concentration of 0.1% of this raw material in skincare products, such as facial and body creams, the products will possess the aforementioned attributes. DETAILED DESCRIPTION

[0017] According to the present invention, the process for obtaining raw material from Lilium orientalis Stargazer waste first comprises separating the petal waste, previously used for essential oil extraction, a process known as enflaurage, and the rest of the plant into parts (stems, pistils and anthers) to be separately conveyed for drying.

[0018] Thus, initially the fresh petals undergo the enfleurage process, a process for extracting essential oils, where said petals are placed in trays and a vegetable fat is placed on the lids in the proportion of 1 gram of vegetable fat per lily petal. The place where these closed trays are kept is air-conditioned, in the range of 30°C to 35°C, so that the essential oil evaporates and Petition 870250005852, dated 01 / 24 / 2025, page 16 / 25 6 / 11 fixes itself in vegetable fat. This process takes place over 48 hours, so that the maximum amount of essential oil is extracted from the petals without any contact between the fat and the petals. Following this, the fat undergoes a distillation process to separate the essential oil from the rest of the material, which is then directed to other processes. Finally, the residual petals, or petal residue, that would otherwise be discarded, are dried, as are the remaining parts of the lily.

[0019] The drying process is carried out in a conventional oven at a temperature ranging from 50°C to 70°C (since temperatures higher than 70°C can degrade the material) until the maximum moisture content of the stems, pistils and anthers is up to 10%, preferably a maximum moisture content of 6% for the petal, stem and filament residues, and a maximum moisture content of 10% for the anthers (since even after 3 days, it is not possible to lower the moisture content below this value in this part of the lily).

[0020] These moisture contents are determined in the present invention as ideal so that there are no interferences in the raw material and so that there is not enough moisture to cause contamination with fungi, for example.

[0021] At this stage of the drying process, after 3 days the moisture content is measured and if the moisture content is above the specified level, the petal residue (after essential oil extraction), stems, pistils and anthers are returned to the oven to continue drying.

[0022] After the drying process, these parts of petal, stem, pistil and anther residues of Lilium orientalis Stargazer are subjected to a hydroalcoholic extraction process, with the solvent composition being 30% to 70% alcohol, preferably 50%, and the proportion of total plant residues to solvent being equal parts.

[0023] To determine the parameters of the present invention, various proportions between the parts of the lily were analyzed until the optimum proportion was reached, always with the petal and filament residues (2 parts each) in a greater proportion than the anthers and stems (0.5 parts each), aiming to obtain the best composition of the raw material from the residues of Lilium orientalis Stargazer. Petition 870250005852, dated 01 / 24 / 2025, page 17 / 25 7 / 11

[0024] This extraction process takes place over 10 hours at room temperature. After the specified time, the mixture is filtered to remove solid residues and is then concentrated under reduced pressure and without altering the temperature.

[0025] The concentrated product receives the addition of glycerin (10:1 product:glycerin), its pH is adjusted to the desired range of 3.5 to 4.0 with citric acid, and then it is filtered again to obtain a material free of solids.

[0026] Finally, the raw material from lily waste with antioxidant action comprises the antioxidant composition presented in Table 2. Table 2 Raw material concentration (mg / mL) Polyphenols (mg gallic acid equivalent / g of raw material) Total Flavonoids (g / mL) 4,460 3,282 14,600

[0027] For this hydroalcoholic extraction process, water and alcohol are used in a proportion of 30% to 70% alcohol, preferably 50%, with the remainder being water and a predefined quantity of parts of the Lilium orientalis Stargazer lily. Thus, according to the present invention, the composition resulting from the process of obtaining raw material from Lilium orientalis Stargazer, which comprises petal residues previously used for essential oil extraction, and other residues composed of stems, pistils, and anthers, has the following physicochemical characteristics: an opaque solution at 20°C; a pH of 3.5 to 4.0; a flash point greater than or equal to 100°C; a density at 20°C of 1.00 to 1.10; and a refractive index at 20°C of 1.30 to 1.45.These characteristics are inherent and serve as a basis for the production of new batches of this raw material, a requirement of the quality control area in order to achieve the essential attributes for the present invention.

[0028] Based on the antioxidant activity and in vitro efficacy tests to which the raw material obtained by the process described above was subjected, it was proven that the use of 0.1% of this ingredient, which can be employed in various variations of cosmetic compositions already known in the state of the art, Petition 870250005852, dated 01 / 24 / 2025, page 18 / 25 8 / 11 exhibits superior antioxidant activity compared to Vitamin C, in addition to providing benefits such as cell regeneration and renewal, cell detoxification, protection against oxidative stress and free radicals and pollutants, contributes to the integrity of the skin barrier, prevents water loss from the skin, and increases the expression of genes that stimulate the production of multiple collagens in the skin. The attributes highlighted above are based on the results of the ORAC test for antioxidant activity, in which a sample of the raw material was diluted in a 1:2000 ratio with phosphate buffer pH 7.4 and analyzed in triplicate using the ORAC method, with a Trolox standard and the analytical curve established in the range of 0.04 to 0.12 µM / mL. Readings were taken at wavelengths of 485 nm and 520 nm. The interval between measurements was 30 seconds for 90 minutes, totaling 181 measurement cycles. The first 4 cycles were used to determine the background value.The sample evaluated showed a result of 160.5 Trolox equivalents, meaning that 1 µL of the raw material has an antioxidant action equivalent to 160.5 µM of Trolox, a stable and water-soluble form of vitamin E. According to literature data, 1 µM of Trolox has an antioxidant action equivalent to 1.9 µM of Vitamin C. Therefore, it was concluded that 1 mL of the present raw material is equivalent to 304.95 mM or 53.71 grams of Vitamin C.

[0029] The in vitro efficacy potential of lily raw material was determined through genetic sequencing (RNA-seq) testing in a 3D skin model, which mimics the structure and function of human skin, representing a promising solution for conducting highly complex experiments. Furthermore, these models can be used to evaluate the complex molecular interactions that modulate skin phenotype after exposure to chemical compounds. It is in this context that genetic sequencing, and more specifically RNA-Seq, demonstrates its importance in this evaluation role. For this test, concentration conditions of 0.05% and 0.1% of the raw material were defined, with the application of 25 µL of sample to each 3D skin model for a period of 24 hours. Each independent experiment was performed in triplicate, which constituted a pool of samples used in the sequencing step. This Petition 870250005852, dated 01 / 24 / 2025, page 19 / 25 The final step, 9 / 11, involves RNA extraction from the sample, conversion to cDNA, high-throughput sequencing, and mapping of the reads to a reference genome (Homo sapiens). Data analysis allowed for the quantification of gene expression, identification of differentially expressed genes, and investigation of transcriptional regulatory networks. Analyzing differentially expressed genes, the lowest concentration of the raw material (0.05%) modulated only 16 genes, making it impossible to attribute any cosmetic benefit after treatment in the 3D skin model at this concentration. However, the highest concentration tested (0.1%) significantly modulated the expression of 804 genes, with 273 showing reduced (downregulated) expression and 531 showing increased (upregulated) gene expression. When evaluating the altered genes, correlations were made with the potential cosmetic attributes associated with the raw material, as shown in Table 3. Table 3 Genes Function % increase in expression Attribute CLDN7 Important for skin barrier function 110% Helps maintain the integrity of the skin barrier; Prevention of water loss. COL4A2 Important structural components of the skin basement membrane 99% 99% increase in collagen production stimulation. COL4A1 Important structural components of the skin basement membrane 96% 96% increase in collagen production stimulation. ABCC10 Protects against oxidative stress, which can damage the skin 90% Cellular detoxification; Antioxidant; Protection against oxidative stress; Protection against free radicals and pollutants. FDXR Protects against oxidative stress, which can damage the skin 84% Cellular detoxification; Antioxidant; Protection against oxidative stress; Protection against free radicals and pollutants.MT2A protects against oxidative stress, which can damage the skin. 81% Cellular detoxification; Antioxidant; Protection against oxidative stress; Protection against free radicals and pollutants. Petition 870250005852, dated 01 / 24 / 2025, page 20 / 25 10 / 11 ITGB4 Essential for adhesion between epidermal cells and the basement membrane 61% Helps maintain the integrity of the skin barrier; Prevention of water loss. COL7A1 Essential for the adhesion of the epidermis to the dermis 56% 56% increase in collagen production stimulation. GSTP1 Protects against oxidative stress, which can damage the skin 56% Cellular detoxification; Antioxidant; Protection against oxidative stress; Protection against free radicals and pollutants. HSPG2 Important for the structure and function of the skin's basement membrane 52% Acts in processes involved in cell regeneration. TGFB1 Crucial role in wound healing, inflammation and collagen production 50% Cellular regeneration; cell renewal. KRT5 Essential for the strength and integrity of the epidermis 32% Contributes to the integrity of the skin barrier; Cellular regeneration and renewal.

[0030] As examples of compositions comprising the raw material object of the invention, facial toner and intensive moisturizing cream compositions are presented, examples 1 and 2, respectively. These comprise the amount of 0.1%, sufficient to provide the proven benefits described above. Table 4 - Example 1 Ingredient Concentration (%) COSMETIC RAW MATERIAL FROM LILY RESIDUES 0.1 SODIUM POLYACRYLATE / XYLITOL / STEARATE GL 2.5 WATER 93.6 DISODIUM EDETATE 0.1 GLYCEROL 1 ETHYLHEXYLGLYCERIN 0.5 PURE PHENOXYETHANOL 0.6 Petition 870250005852, dated 01 / 24 / 2025, page 21 / 25 11 / 11 DICAPRILYL CARBONATE 0.5 ESS LILY EXT IFRA 49 RW3 HYPER 2 0.6 CAPRIC / CAPRIL TRIGLYCERIDES 0.5 Table 5 - Example 2 Ingredient Concentration (%) COSMETIC RAW MATERIAL FROM LILY RESIDUES 0.1 SODIUM POLYACRYLATE 1 WATER 82.7 GLYCEROL 3 ​​ALKYL BENZOATE Cl2-15 3 PURIFIED SWEET ALMOND OIL 4 PURE PHENOXYETHANOL 0.6 DICAPRYLLYL CARBONATE 4 BETAINE 0.5 ORGANIC SODIUM GLUCONATE 0.2 ESSENCE LILY EXT IFRA 49 RW3 HYPER 2 0.6 HYDROXYACETOPHENONE 0.3

[0031] This invention is not limited to the representations of the examples, that is, it is not limited to the ingredients and quantities mentioned and should be understood in its broad scope. Many modifications and other representations of the invention will come to mind of one skilled in the art to which this invention pertains, having the benefit of the teaching set forth in the preceding descriptions. Petition 870250005852, dated 01 / 24 / 2025, page 22 / 25

Claims

1 / 2 CLAIMS 1.) “COSMETIC RAW MATERIAL FROM LILY RESIDUES”, characterized by comprising: 90% concentrated extraction residue composed of 3,282 mg of polyphenols / g of raw material and 14,600 μg / mL of total flavonoids; and 10% glycerin. 2.) “COSMETIC RAW MATERIAL FROM LILY RESIDUES”, according to claim 1, characterized by comprising antioxidant activity equivalent to 160.5 mM of Trolox in each mL. 3.) “PROCESS FOR OBTAINING COSMETIC RAW MATERIAL FROM LILY WASTE”, characterized by comprising the following steps: separating the petals of Lilium orientalis Stargazer for the extraction of essential oil, where said petals are placed in trays with lids containing vegetable fat in the proportion of 1 gram of vegetable fat per lily petal, at a temperature of 30°C to 35°C, for 48 hours; the fat is then distilled and the residual petals are dried, as well as the remaining parts of the lily, in a conventional oven at a temperature ranging from 50°C to 70°C, until the maximum moisture content of the stem, pistil and anther parts is 10%, preferably a maximum moisture content of 6% for the petal, stem and filament waste, and a maximum moisture content of 10%;After the drying process, the petal, anther, and stem residues (in a 2:2:0.5:0.5 ratio) receive, in an amount equal to their weight, a hydroalcoholic solvent composed of 30% to 70% alcohol, preferably 50%; this step occurs for 10 hours at room temperature, followed by filtration and concentration under reduced pressure, without altering the temperature; finally, the product receives the addition of glycerin, in a 10:1 ratio, respectively, and its pH is adjusted to the range of 3.5 to 4.0 with citric acid followed by filtration. 4.) “USE OF COSMETIC RAW MATERIAL FROM LILY RESIDUES” understood to contain 90% residue from the extraction composed of 3,282 mg of polyphenols / g of raw material and 14,600 μg / mL of total flavonoids; and 10% glycerin, characterized by the application of 0.1% of said cosmetic raw material from lily residues in cosmetic compositions for cell regeneration and renewal, cell detoxification, protection against oxidative stress and against free radicals and pollutants, contribution to the integrity of the skin barrier, prevention of water loss from the skin and increased stimulation of the production of multiple skin collagens. Petition 870250005852, dated 01 / 24 / 2025, page 24 / 25