Extraction process of sarcodia montagneana and application of sarcodia montagneana in strengthening and toughening hair quality in hair products

Abstract

The invention relates to an extraction process of sarcodia montagneana and application of sarcodia montagneana in strengthening and toughening hair quality in hair products, and belongs to the technical field of algae extraction. The method comprises the following steps: preliminarily extracting sarcodia montagneana through a water phase, and centrifuging and filtering a mixed solution to obtain supernate and filter residues; carrying out ammonium sulfate fractional precipitation on the supernate, dialyzing and desalting, and freeze-drying to obtain phycobiliprotein; and carrying out supercritical CO2 fluid extraction on the filter residue by adopting a lactic acid solution entrainer, and carrying out membrane concentration and drying to obtain the sarcodia montagneana polysaccharide. The phycobiliprotein and sarcodia montagneana polysaccharide are fermented by lactobacillus, and the product is rich in lactic acid, amino acid and other micromolecular active ingredients, can permeate into the hair more easily, and has a deep nourishing effect.

Description

Technical Field

[0001] The present invention belongs to the technical field of algae extraction, and relates to an extraction process of Sargassum fusiforme and its application in strengthening hair quality in hair products. Background Art

[0002] Sargassum fusiforme is a unique alga growing in the ocean, rich in various bioactive components. Its special living environment endows it with abundant nutrients, such as phycobiliprotein, Sargassum fusiforme polysaccharide, etc. Phycobiliprotein not only plays an important role in photosynthesis, but also has unique optical properties, and has shown certain application values in the fields of food, medicine, etc. And Sargassum fusiforme polysaccharide has a complex structure and diverse functions, containing various monosaccharides and glycosidic bonds, which provides a broad space for the research on its biological activities.

[0003] The health and appearance of hair have always been the focus of people's attention. The main problems of hair include dryness, easy breakage, damaged hair cuticles, and lack of luster, etc. Various components contained in Sargassum fusiforme have significant potential for improving hair quality. Sargassum fusiforme polysaccharide has various effects such as antioxidant, anti-inflammatory and antibacterial. In hair care, the antioxidant effect can effectively resist the damage of free radicals to hair, slow down hair aging, and keep hair energetic; the anti-inflammatory effect can soothe scalp inflammation and reduce the generation of dandruff; the antibacterial effect helps to maintain a healthy microbial environment on the scalp and prevent the growth of harmful bacteria. At the same time, other components in Sargassum fusiforme may interact with the keratin of hair, enhance the toughness of hair, improve the combability of hair, and repair damaged hair cuticles, so that the hair is more smooth, strong and shiny.

[0004] However, at present, in the field of hair care products, there are still many deficiencies in the research on the extraction process of Sargassum fusiforme and its application in hair products. Existing extraction processes often cannot extract the key active components in Sargassum fusiforme efficiently and with high purity, resulting in higher extraction costs and lower utilization rates of active components. In terms of hair product formula design, although there are many chemical components used in hair care, there is still a lack of systematic research on how to scientifically and reasonably mix the extracts of Sargassum fusiforme with traditional hair product components to exert its maximum efficacy. This limits the application of Sargassum fusiforme in hair products and cannot fully display its unique hair care advantages. Therefore, developing an efficient extraction process of Sargassum fusiforme and deeply studying its application in hair products have important practical significance and market value. Summary of the Invention

[0005] The present invention relates to an extraction process of Sargassum fusiforme algae and its application in strengthening hair quality in hair products, belonging to the technical field of algae extraction. In the present invention, Sargassum fusiforme algae is preliminarily extracted in the aqueous phase, and then the mixed solution is centrifuged and filtered to obtain the supernatant and the filter residue. The supernatant is subjected to ammonium sulfate fractional precipitation, dialysis desalting, and freeze-drying to obtain phycobiliprotein; the filter residue is subjected to supercritical CO2 fluid extraction using a lactic acid solution entrainer, and then through membrane concentration and drying to obtain Sargassum fusiforme polysaccharide. The phycobiliprotein and Sargassum fusiforme polysaccharide are fermented by Lactobacillus, and the product is rich in small molecule active ingredients such as lactic acid and amino acids, which are more likely to penetrate into the hair strands and play a deep nourishing effect when used.

[0006] The object of the present invention can be achieved by the following technical solutions:

[0007] An extraction process of Sargassum fusiforme algae, comprising the following steps:

[0008] (1) After mixing Sargassum fusiforme algae powder with deionized water, preliminary extraction in the aqueous phase is carried out by gradient temperature rise combined with ultrasonic treatment;

[0009] (2) The mixed solution in step (1) is centrifuged and filtered to obtain the supernatant and the filter residue. The supernatant is subjected to ammonium sulfate fractional precipitation, and then through dialysis desalting and freeze-drying to obtain phycobiliprotein;

[0010] (3) The filter residue obtained in step (2) is subjected to supercritical CO2 fluid extraction using a lactic acid solution entrainer;

[0011] (4) The extract is centrifuged, membrane concentrated, filtered through a 0.22 μm sterile filter membrane, and then spray-dried to obtain Sargassum fusiforme polysaccharide.

[0012] As a preferred technical solution of the present invention, the mass ratio of the Sargassum fusiforme algae powder to deionized water in step (1) is 1:10 - 20; the gradient temperature rise is to heat the mixed solution of Sargassum fusiforme algae powder and deionized water to 45 - 55 °C and keep it warm for 40 - 80 min, then raise the temperature to 60 - 70 °C and keep it warm for 100 - 140 min, and then raise the temperature to 75 - 85 °C and keep it warm for 40 - 80 min.

[0013] As a preferred technical solution of the present invention, the ammonium sulfate fractional precipitation in step (2) is to add ammonium sulfate to the supernatant at a rate of 5 g / min to 40% saturation, stand at 4 °C for 12 h, then centrifuge to remove the precipitate of impurity proteins, continue to add ammonium sulfate to 60% saturation by increasing 5% saturation every 30 min, and centrifuge to obtain the precipitate, which is resuspended with an equal mass of 20 mM PBS with a pH of 7.0.

[0014] As a preferred technical solution of the present invention, the mass ratio of the filter residue to the entrainer in step (3) is 1:1 - 3; the supercritical CO2 fluid extraction pressure is 31 - 33 MPa, the temperature is 48 - 52 °C, the CO2 flow rate is 20 - 30 L / h, the extraction time is 90 - 150 min, and the static impregnation time is 20 - 40 min; the entrainer is a 3 - 8 wt% lactic acid solution.

[0015] As a preferred technical solution of the present invention, the centrifugation speed in step (4) is 10000 - 15000 rpm, and the centrifugation time is 20 - 40 min; the membrane concentration is: ultrafiltration through a 10 kDa hollow fiber membrane to retain polysaccharides, and the pressure is set to 1 - 1.5 MPa for concentration until the solid content is 20 - 50%; the inlet air temperature of the spray drying is 160 - 200 °C, and the outlet air temperature is 80 - 90 °C.

[0016] As a preferred technical solution of the present invention, the phycobiliprotein and polysaccharide of Sargassum fusiforme extracted are applied to hair products.

[0017] As a preferred technical solution of the present invention, the hair product comprises the following raw materials in parts by weight: 70 - 80 parts of deionized water, 8 - 12 parts of sodium cocoyl glutamate, 1.5 - 8 parts of the fermentation product of phycobiliprotein and polysaccharide of Sargassum fusiforme, 2 - 3 parts of hyaluronic acid, 1 - 3 parts of rose essential oil, 1 - 2 parts of chamomile extract, 0.5 - 1 part of seaweed gum, and 0.5 - 1 part of vitamin E.

[0018] As a preferred technical solution of the present invention, the hair product comprises the following preparation steps:

[0019] S1. Heat the deionized water to 60 - 80 °C, add seaweed gum, stir until completely dissolved, add sodium cocoyl glutamate, control the temperature at about 40 - 60 °C, and stir until completely dissolved;

[0020] S2. When the temperature drops to 35 - 45 °C, add the fermentation product of phycobiliprotein and polysaccharide of Sargassum fusiforme, hyaluronic acid, and rose essential oil, stir evenly, and add chamomile extract and stir evenly;

[0021] S3. Adjust the pH value to 4.5 - 5.5 with lactic acid, add vitamin E, and stir evenly.

[0022] As a preferred technical solution of the present invention, the preparation process of the fermentation product of phycobiliprotein and polysaccharide of Sargassum fusiforme includes: activating and culturing Lactobacillus in MRS medium at 30 - 37 °C for 18 - 24 h, inoculating it into the fermentation medium at 5 - 10% and fermenting at 30 - 37 °C for 24 - 48 h, then homogenizing and crushing, centrifuging to remove residues, and drying to obtain the fermentation product;

[0023] Among them, the fermentation medium is: 10 - 20 g / L glucose, 5 - 10 g / L yeast powder, 10 - 20 g / L soybean powder, 2 - 5 g / L seaweed powder, 0.5 - 5 g / L phycobiliprotein, 0.5 - 5 g / L Sargassum fusiforme polysaccharide, and the balance is deionized water.

[0024] Advantages of the present invention:

[0025] (1) The present invention first uses a combined method of gradient heating and ultrasonic treatment for preliminary extraction, which not only improves the dissolution efficiency of Sargassum fusiforme components but also maintains the stability of its bioactive components. The combination of ammonium sulfate fractional precipitation method and supercritical CO2 fluid extraction technology using lactic acid solution entrainer makes the extraction process of phycobiliprotein and Sargassum fusiforme polysaccharide more efficient and accurate. Finally, techniques such as dialysis and membrane concentration are used for fine treatment, effectively removing impurities, improving the purity and activity of the final product, and making its application effect in skin care and hair products more significant. This process improves the extraction efficiency and component activity of Sargassum fusiforme while ensuring environmental friendliness and sustainability.

[0026] (2) Phycobiliprotein and Sargassum fusiforme polysaccharide have the functions of antioxidant, anti-inflammatory, and repairing hair cuticles, and can effectively improve the gloss, toughness, and combability of hair. By combining ingredients such as amino acid surfactants, cationic polymers, and plant essential oils, the formula not only enhances the moisturizing effect of hair but also repairs hair damage caused by external environment or chemical treatment. The synergistic effect of this innovative formula can improve the health level of hair, improve hair quality, and increase the elasticity and gloss of hair at the same time. Specific embodiments

[0027] To further elaborate on the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the following examples are used to describe in detail the specific embodiments, structures, features, and their effects according to the present invention.

[0028] In the following examples and comparative examples, Sargassum fusiforme was purchased from Supervision Biotechnology Development Co., Ltd.; rose essential oil was purchased from Bolly Aromatic Medicine Technology Co., Ltd., with the product number PER0601; tea tree essential oil was purchased from Qingyuan Huiwen Spice Co., Ltd.; chamomile extract was purchased from Shaanxi Xinyanghe Biotechnology Co., Ltd.; alginate was purchased from Meiyi Pharmacy Flagship Store; vitamin E was purchased from Shandong Kangrong Pharmaceutical Co., Ltd.; yeast powder was purchased from Jinan Yuncheng Biotechnology Co., Ltd.; soybean powder was purchased from Weimao Biotechnology Co., Ltd., with the product number 6686681041; seaweed powder was purchased from Hengde Biotechnology Co., Ltd.; MRS medium was purchased from Qingdao Haibo Biotechnology.

[0029] Example 1

[0030] An extraction process of Sargassum fusiforme includes the following steps:

[0031] (1) Mix the Sargassum fusiforme powder with deionized water, and then conduct preliminary aqueous extraction by using gradient temperature rise combined with ultrasonic treatment.

[0032] (2) Centrifuge and filter the mixed solution in step (1) to obtain the supernatant and the residue. Perform ammonium sulfate fractional precipitation on the supernatant, and then desalt by dialysis and freeze-dry to obtain phycobiliprotein.

[0033] (3) Use a lactic acid solution entrainer to perform supercritical CO2 fluid extraction on the residue obtained in step (2).

[0034] (4) Centrifuge the extraction solution, concentrate by membrane, filter through a 0.22 μm sterile filter membrane, and then spray-dry to obtain Sargassum fusiforme polysaccharide.

[0035] In step (1), the mass ratio of the Sargassum fusiforme powder to deionized water is 1:15; the gradient temperature rise is to heat the mixed solution of the Sargassum fusiforme powder and deionized water to 50 °C and keep it warm for 60 min, then raise the temperature to 65 °C and keep it warm for 120 min, and then raise the temperature to 80 °C and keep it warm for 60 min.

[0036] The ammonium sulfate fractional precipitation in step (2) is to add ammonium sulfate to the supernatant at a rate of 5 g / min until the saturation degree reaches 40%, let it stand at 4 °C for 12 h, then centrifuge to remove the precipitate of impurity proteins, continue to add ammonium sulfate at a rate of increasing 5% saturation degree every 30 min until the saturation degree reaches 60%, and centrifuge to obtain the precipitate and resuspend it with an equal mass of 20 mM PBS with a pH of 7.0.

[0037] In step (3), the mass ratio of the residue to the entrainer is 1:2; the pressure of the supercritical CO2 fluid extraction is 32 MPa, the temperature is 50 °C, the CO2 flow rate is 25 L / h, the extraction time is 120 min, and the static impregnation time is 30 min; the entrainer is a 5 wt% lactic acid solution.

[0038] In step (4), the centrifugation speed is 12000 rpm and the centrifugation time is 30 min; the membrane concentration is: ultrafiltrate and retain the polysaccharide through a 10 kDa hollow fiber membrane, and set the pressure to 1.2 MPa to concentrate until the solid content reaches 35%; the inlet air temperature of the spray drying is 180 °C and the outlet air temperature is 85 °C.

[0039] The phycobiliprotein and Sargassum fusiforme polysaccharide extracted from Sargassum fusiforme are applied to hair products.

[0040] The hair product comprises the following raw materials in parts by weight: 75 parts of deionized water, 10 parts of sodium cocoyl glutamate, 5 parts of the fermentation product of phycobiliprotein and Sargassum fusiforme polysaccharide, 2.5 parts of hyaluronic acid, 2 parts of rose essential oil, 1.5 parts of chamomile extract, 0.7 part of alginate and 0.7 part of vitamin E.

[0041] The hair product comprises the following preparation steps:

[0042] S1. Heat deionized water to 70°C, add alginate, stir until completely dissolved, add sodium cocoyl glutamate, control the temperature at about 50°C, and stir until completely dissolved;

[0043] S2. When the temperature drops to 40°C, add phycobiliprotein, fermentation product of Sargassum fusiforme polysaccharide, hyaluronic acid and rose essential oil, stir evenly, and add chamomile extract and stir evenly;

[0044] S3. Adjust the pH value to 5.0 with lactic acid, add vitamin E, and stir evenly.

[0045] The preparation process of the phycobiliprotein and the fermentation product of Sargassum fusiforme polysaccharide includes: activating and culturing Lactobacillus in MRS medium at 35°C for 21 h, inoculating at 8% into the fermentation medium, fermenting at 35°C for 36 h, then performing homogenization and crushing, centrifuging to remove residues, and drying to obtain the fermentation product;

[0046] The fermentation medium is: 16 g / L glucose, 8 g / L yeast powder, 16 g / L soybean powder, 4 g / L seaweed powder, 3 g / L phycobiliprotein, 3 g / L Sargassum fusiforme polysaccharide, and the balance is deionized water.

[0047] Example 2

[0048] An extraction process of Sargassum fusiforme algae includes the following steps:

[0049] (1) After mixing Sargassum fusiforme algae powder with deionized water, perform preliminary aqueous phase extraction by gradient heating combined with ultrasonic treatment;

[0050] (2) Centrifuge and filter the mixed solution in step (1) to obtain the supernatant and filter residue. Perform ammonium sulfate fractional precipitation on the supernatant, then desalt by dialysis and freeze-dry to obtain phycobiliprotein;

[0051] (3) Use the filter residue obtained in step (2) for supercritical CO2 fluid extraction with a lactic acid solution entrainer;

[0052] (4) Centrifuge the extract, perform membrane concentration, filter through a 0.22 μm sterile filter membrane, and then spray-dry to obtain Sargassum fusiforme polysaccharide.

[0053] In step (1), the mass ratio of the Sargassum fusiforme algae powder to deionized water is 1:10; the gradient heating is to heat the mixed solution of Sargassum fusiforme algae powder and deionized water to 45°C and keep it warm for 40 min, then raise the temperature to 60°C and keep it warm for 100 min, and then raise the temperature to 75°C and keep it warm for 40 min.

[0054] The ammonium sulfate fractional precipitation described in step (2) is to add ammonium sulfate to the supernatant at a rate of 5 g / min until the saturation reaches 40%, stand at 4°C for 12 h, then centrifuge to remove the precipitate of impurity proteins. Continue to add ammonium sulfate to increase the saturation by 5% every 30 min until the saturation reaches 60%. The obtained precipitate is resuspended with an equal mass of 20 mM PBS with a pH of 7.0.

[0055] The mass ratio of the filter residue to the entrainer in step (3) is 1:1; the supercritical CO2 fluid extraction pressure is 31 MPa, the temperature is 48 - 52°C, the CO2 flow rate is 20 L / h, the extraction time is 90 min, and the static impregnation time is 20 min; the entrainer is a solution containing 3 wt% lactic acid.

[0056] The centrifugation speed in step (4) is 10,000 rpm and the centrifugation time is 20 min; the membrane concentration is as follows: ultrafiltration through a 10 kDa hollow fiber membrane to retain polysaccharides, and the pressure is set to 1 MPa for concentration until the solid content reaches 20%; the inlet air temperature for spray drying is 160°C and the outlet air temperature is 80°C.

[0057] The phycobiliprotein and polysaccharide extracted from Sargassum fusiforme are applied to hair products.

[0058] The hair products include the following raw materials in parts by weight: 70 parts of deionized water, 8 parts of sodium cocoyl glutamate, 1.5 parts of the fermentation product of phycobiliprotein and polysaccharide from Sargassum fusiforme, 2 parts of hyaluronic acid, 1 part of rose essential oil, 1 part of chamomile extract, 0.5 part of alginate and 0.5 part of vitamin E.

[0059] The hair products include the following preparation steps:

[0060] S1. Heat the deionized water to 60°C, add alginate, stir until completely dissolved, then add sodium cocoyl glutamate, and control the temperature at about 40°C and stir until completely dissolved;

[0061] S2. When the temperature drops to 35°C, add the fermentation product of phycobiliprotein and polysaccharide from Sargassum fusiforme, hyaluronic acid and rose essential oil, and stir evenly, then add chamomile extract and stir evenly;

[0062] S3. Adjust the pH value to 4.5 with lactic acid, add vitamin E, and stir evenly.

[0063] As a preferred technical solution of the present invention, the preparation process of the fermentation product of phycobiliprotein and polysaccharide from Sargassum fusiforme includes: activating and culturing Lactobacillus in MRS medium at 30°C for 18 h, inoculating into the fermentation medium at 5 - 10% and fermenting at 30°C for 24 h, then homogenizing, crushing, centrifuging to remove residues and drying to obtain the fermentation product;

[0064] Among them, the fermentation medium is: 10 g / L glucose, 5 g / L yeast powder, 10 g / L soybean powder, 2 g / L seaweed powder, 0.5 g / L phycobiliprotein, 0.5 g / L Sargassum fusiforme polysaccharide, and the balance is deionized water.

[0065] Example 3

[0066] An extraction process of Sargassum fusiforme algae includes the following steps:

[0067] (1) After mixing Sargassum fusiforme algae powder with deionized water, preliminary aqueous extraction is carried out by gradient heating combined with ultrasonic treatment;

[0068] (2) The mixed solution in step (1) is centrifuged and filtered to obtain the supernatant and the filter residue. The supernatant is subjected to ammonium sulfate fractional precipitation, and then dialyzed to remove salt and freeze-dried to obtain phycobiliprotein;

[0069] (3) The filter residue obtained in step (2) is subjected to supercritical CO2 fluid extraction using a lactic acid solution entrainer;

[0070] (4) The extract is centrifuged, membrane concentrated, filtered through a 0.22 μm sterile filter membrane, and then spray-dried to obtain Sargassum fusiforme polysaccharide.

[0071] In step (1), the mass ratio of the Sargassum fusiforme algae powder to deionized water is 1:10 - 20; the gradient heating is to heat the mixed solution of Sargassum fusiforme algae powder and deionized water to 55 °C and keep it warm for 80 min, then raise the temperature to 70 °C and keep it warm for 140 min, and then raise the temperature to 85 °C and keep it warm for 80 min.

[0072] The ammonium sulfate fractional precipitation in step (2) is to add ammonium sulfate to the supernatant at a rate of 5 g / min to 40% saturation, stand at 4 °C for 12 h, then centrifuge to remove the precipitate of impurity proteins, continue to add ammonium sulfate to 60% saturation by increasing 5% saturation every 30 min, and the precipitate obtained by centrifugation is resuspended with an equal mass of 20 mM PBS with a pH of 7.0.

[0073] In step (3), the mass ratio of the filter residue to the entrainer is 1:3; the pressure of the supercritical CO2 fluid extraction is 33 MPa, the temperature is 52 °C, the CO2 flow rate is 30 L / h, the extraction time is 150 min, and the static impregnation time is 40 min; the entrainer is 8 wt% lactic acid solution.

[0074] In step (4), the centrifugation speed is 15000 rpm and the centrifugation time is 40 min; the membrane concentration is: ultrafiltration through a 10 kDa hollow fiber membrane to retain polysaccharides, and the pressure is set to 1.5 MPa to concentrate to a solid content of 50%; the inlet air temperature of the spray drying is 200 °C and the outlet air temperature is 90 °C.

[0075] The phycobiliprotein and polysaccharide of Sargassum fusiforme extracted are applied to hair products.

[0076] The hair products comprise the following raw materials in parts by weight: 80 parts of deionized water, 12 parts of sodium cocoyl glutamate, 8 parts of the fermentation product of phycobiliprotein and polysaccharide of Sargassum fusiforme, 3 parts of hyaluronic acid, 3 parts of rose essential oil, 2 parts of chamomile extract, 1 part of seaweed glue and 1 part of vitamin E.

[0077] The hair products comprise the following preparation steps:

[0078] S1. Heat the deionized water to 80 °C, add seaweed glue, stir until completely dissolved, add sodium cocoyl glutamate, control the temperature at about 60 °C, and stir until completely dissolved;

[0079] S2. When the temperature drops to 45 °C, add the fermentation product of phycobiliprotein and polysaccharide of Sargassum fusiforme, hyaluronic acid and rose essential oil, stir evenly, and add chamomile extract and stir evenly;

[0080] S3. Adjust the pH value to 5.5 with lactic acid, add vitamin E, and stir evenly.

[0081] As a preferred technical solution of the present invention, the preparation process of the fermentation product of phycobiliprotein and polysaccharide of Sargassum fusiforme includes: activating and culturing Lactobacillus in MRS medium at 37 °C for 24 h, inoculating into the fermentation medium at 10% and fermenting at 37 °C for 48 h, then performing homogenization and crushing, centrifuging to remove residues, and drying to obtain the fermentation product;

[0082] The fermentation medium is: 20 g / L glucose, 10 g / L yeast powder, 20 g / L soybean powder, 5 g / L seaweed powder, 5 g / L phycobiliprotein, 5 g / L polysaccharide of Sargassum fusiforme, and the balance is deionized water.

[0083] Example 4

[0084] An extraction process of Sargassum fusiforme includes the following steps:

[0085] (1) After mixing Sargassum fusiforme powder with deionized water, perform preliminary aqueous phase extraction by gradient temperature rise combined with ultrasonic treatment;

[0086] (2) Centrifuge and filter the mixed solution in step (1) to obtain the supernatant and filter residue. Perform ammonium sulfate fractional precipitation on the supernatant, then desalt by dialysis and freeze-dry to obtain phycobiliprotein;

[0087] (3) Use lactic acid solution entrainer to perform supercritical CO2 fluid extraction on the filter residue obtained in step (2);

[0088] (4) Centrifuge the extract, perform membrane concentration, filter through a 0.22 μm sterile filter membrane, and then spray-dry to obtain polysaccharide of Sargassum fusiforme.

[0089] In step (1), the mass ratio of the Sargassum fusiforme powder to deionized water is 1:12; the gradient heating is to heat the mixture of the Sargassum fusiforme powder and deionized water to 42 °C and keep it warm for 50 min, then heat it up to 68 °C and keep it warm for 110 min, and then heat it up to 78 °C and keep it warm for 70 min.

[0090] In step (2), the ammonium sulfate fractional precipitation is to add ammonium sulfate to the supernatant at a rate of 5 g / min until the saturation reaches 40%, let it stand at 4 °C for 12 h, then centrifuge to remove the precipitate of impurity proteins, continue to add ammonium sulfate to increase the saturation by 5% every 30 min until the saturation reaches 60%, and centrifuge to obtain the precipitate, which is resuspended with an equal mass of 20 mM PBS with a pH of 7.0.

[0091] In step (3), the mass ratio of the filter residue to the entrainer is 1:1; the supercritical CO2 fluid extraction pressure is 31 MPa, the temperature is 51 °C, the CO2 flow rate is 22 L / h, the extraction time is 100 min, and the static impregnation time is 25 min; the entrainer is a 4 wt% lactic acid solution.

[0092] In step (4), the centrifugation speed is 11000 rpm and the centrifugation time is 25 min; the membrane concentration is: ultrafiltration through a 10 kDa hollow fiber membrane to retain polysaccharides, and the pressure is set to 1.2 MPa to concentrate until the solid content reaches 30%; the inlet air temperature for spray drying is 170 °C and the outlet air temperature is 88 °C.

[0093] The phycobiliprotein and Sargassum fusiforme polysaccharide extracted from Sargassum fusiforme are applied to hair products.

[0094] The hair products include the following raw materials in parts by weight: 77 parts of deionized water, 9 parts of sodium cocoyl glutamate, 6 parts of the fermentation product of phycobiliprotein and Sargassum fusiforme polysaccharide, 2 parts of hyaluronic acid, 2 parts of rose essential oil, 2 parts of chamomile extract, 1 part of alginate and 1 part of vitamin E.

[0095] The hair products include the following preparation steps:

[0096] S1. Heat the deionized water to 62 °C, add alginate, stir until completely dissolved, add sodium cocoyl glutamate, control the temperature at about 45 °C, and stir until completely dissolved;

[0097] S2. When the temperature drops to 40 °C, add the fermentation product of phycobiliprotein and Sargassum fusiforme polysaccharide, hyaluronic acid and rose essential oil, and stir evenly, then add chamomile extract and stir evenly;

[0098] S3. Adjust the pH value to 4.2 with lactic acid, add vitamin E, and stir evenly.

[0099] The preparation process of the phycobiliprotein and Sargassum fusiforme polysaccharide fermentation product includes: activating and culturing Lactobacillus in MRS medium at 32 °C for 20 h, inoculating it into the fermentation medium at 7% and fermenting at 32 °C for 40 h, then subjecting it to homogenization and crushing, centrifuging to remove residues, and drying to obtain the fermentation product;

[0100] Among them, the fermentation medium is: 12 g / L glucose, 6 g / L yeast powder, 12 g / L soybean powder, 3 g / L seaweed powder, 2 g / L phycobiliprotein, 2 g / L Sargassum fusiforme polysaccharide, and the balance is deionized water.

[0101] Comparative Example 1

[0102] On the basis of Example 1, the gradient heating in step (1) is changed to heating the mixed solution of Sargassum fusiforme powder and deionized water to 50 °C and holding for 240 min, and the rest is the same as Example 1.

[0103] Comparative Example 2

[0104] On the basis of Example 1, the gradient heating in step (1) is changed to heating the mixed solution of Sargassum fusiforme powder and deionized water to 65 °C and holding for 240 min, and the rest is the same as Example 1.

[0105] Comparative Example 3

[0106] On the basis of Example 1, the gradient heating in step (1) is changed to heating the mixed solution of Sargassum fusiforme powder and deionized water to 80 °C and holding for 240 min, and the rest is the same as Example 1.

[0107] Comparative Example 4

[0108] On the basis of Example 1, the entrainer is changed to 5 wt% tea tree essential oil solution, and the rest is the same as Example 1.

[0109] Comparative Example 5

[0110] On the basis of Example 1, phycobiliprotein is not added to the fermentation medium, and the addition amount of Sargassum fusiforme polysaccharide is changed to 6 g / L, and the rest is the same as Example 1.

[0111] Comparative Example 6

[0112] On the basis of Example 1, Sargassum fusiforme polysaccharide is not added to the fermentation medium, and the addition amount of phycobiliprotein is changed to 6 g / L, and the rest is the same as Example 1.

[0113] Performance test:

[0114] Combing property test: Prepare 11 dry hair bundles of the same length (50 cm) and weight (about 16 g). Wash them twice with 3 g of the hair products prepared in Examples 1-4 and Comparative Examples 1-6 respectively; rinse with tap water until there is no foam, and air dry naturally; Test the dry combing property of the treated hair bundles through a tensile tester. First, comb the hair with a plastic comb, then fix the hair sample to be tested with a suitable fixture, place the hair bundle naturally in the middle of the comb. After calibrating and zeroing the instrument, start testing the hair bundle. Stretch the hair bundle at a speed of 300 mm / min for 250 mm. To reduce the measurement error caused by different hair bundles, the same hair bundle is tested 5 times and the average value is taken.

[0115] Tensile strength test: Prepare a dry hair bundle with a length of 50 cm and a weight of 16 g, divide it into 11 equal parts, wash them twice with 0.3 g of the hair products prepared in Examples 1-4 and Comparative Examples 1-6 respectively, rinse with tap water until there is no foam, and air dry naturally; Test the peak value of the tensile strength during the breaking of a single hair in each dry hair bundle through a digital display tensile tester, repeat it ten times and take the average value and record it, which is the hair tensile strength.

[0116]

[0117]

[0118] From the test results, it can be seen that in the present invention, phycobiliprotein is extracted by gradient heating, and lactic acid solution entrainer is used for supercritical CO2 fluid extraction of Sargassum fusiforme polysaccharide. When used in hair products, it can effectively improve the combing property of hair and strengthen hair.

[0119] The above are only the preferred embodiments of the present invention, and do not impose any form of limitation on the present invention. Although the present invention has been disclosed above with preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to equivalent embodiments by using the disclosed technical content within the scope of the technical solution of the present invention. However, as long as it does not depart from the content of the technical solution of the present invention, any indirect modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. An extraction process of Sargassum fusiforme, characterized in that: It includes the following steps: (1) After mixing Gracilaria lemaneiformis powder with deionized water, preliminary aqueous extraction is carried out by gradient heating combined with ultrasonic treatment. (2) The mixed solution in step (1) is centrifuged and filtered to obtain the supernatant and the residue. The supernatant is subjected to ammonium sulfate fractional precipitation, and then desalted by dialysis and freeze-dried to obtain phycobiliprotein. (3) The residue obtained in step (2) is subjected to supercritical CO2 fluid extraction with a lactic acid solution entrainer. (4) The extract is centrifuged, membrane concentrated, filtered through a 0.22 μm sterile filter membrane, and then spray-dried to obtain Gracilaria lemaneiformis polysaccharide.

2. The extraction process of Gracilaria lemaneiformis according to claim 1, characterized in that: In step (1), the mass ratio of Gracilaria lemaneiformis powder to deionized water is 1:10 - 20; the gradient heating is to heat the mixed solution of Gracilaria lemaneiformis powder and deionized water to 45 - 55 °C and keep it warm for 40 - 80 min, then heat it up to 60 - 70 °C and keep it warm for 100 - 140 min, and then heat it up to 75 - 85 °C and keep it warm for 40 - 80 min.

3. The extraction process of Sargassum fusiforme according to claim 1, characterized in that: In step (2), the ammonium sulfate fractional precipitation is to add ammonium sulfate to the supernatant at a rate of 5 g / min until the saturation is 40%, stand still at 4 °C for 12 h, then centrifuge to remove the precipitate of miscellaneous proteins, continue to add ammonium sulfate to increase the saturation by 5% every 30 min until the saturation is 60%, and centrifuge to obtain the precipitate and resuspend it with an equal mass of 20 mM PBS with a pH of 7.

0.

4. The extraction process of Gracilaria lemaneiformis according to claim 1, characterized in that: In step (3), the mass ratio of the residue to the entrainer is 1:1 - 3; the pressure of the supercritical CO2 fluid extraction is 31 - 33 MPa, the temperature is 48 - 52 °C, the CO2 flow rate is 20 - 30 L / h, the extraction time is 90 - 150 min, and the static impregnation time is 20 - 40 min; the entrainer is a 3 - 8 wt% lactic acid solution.

5. The extraction process of Sargassum fusiforme according to claim 1, characterized in that: In step (4), the centrifugation speed is 10000 - 15000 rpm, and the centrifugation time is 20 - 40 min; the membrane concentration is: ultrafiltration and retention of polysaccharides through a 10 kDa hollow fiber membrane, and the pressure is set at 1 - 1.5 MPa to concentrate until the solid content is 20 - 50%; the inlet air temperature of the spray drying is 160 - 200 °C, and the outlet air temperature is 80 - 90 °C.

6. An application of the extraction process of Gracilaria lemaneiformis as described in any one of claims 1-5, characterized in that: The phycobiliprotein and Gracilaria lemaneiformis polysaccharide extracted from Gracilaria lemaneiformis are applied to hair products to help strengthen hair quality.

7. Use of the extraction process of Sargassum fusiforme according to claim 6, characterized in that: The hair product includes the following raw materials in parts by weight: 70 - 80 parts of deionized water, 8 - 12 parts of sodium cocoyl glutamate, 1.5 - 8 parts of the fermentation product of phycobiliprotein and Gracilaria lemaneiformis polysaccharide, 2 - 3 parts of hyaluronic acid, 1 - 3 parts of rose essential oil, 1 - 2 parts of chamomile extract, 0.5 - 1 part of seaweed gum, and 0.5 - 1 part of vitamin E.

8. Use of the extraction process of Sargassum fusiforme according to claim 7, characterized in that: The hair product includes the following preparation steps: S1. Heat the deionized water to 60 - 80 °C, add seaweed gum, stir until completely dissolved, add sodium cocoyl glutamate, control the temperature at about 40 - 60 °C, and stir until completely dissolved. S2. When the temperature drops to 35 - 45 °C, add the fermentation product of phycobiliprotein and Gracilaria lemaneiformis polysaccharide, hyaluronic acid, and rose essential oil, and stir evenly, then add chamomile extract and stir evenly. S3. Adjust the pH value to 4.5 - 5.5 with lactic acid, add vitamin E, and stir evenly.

9. Use of the extraction process of Sargassum fusiforme according to claim 7, characterized in that: The preparation process of the phycobiliprotein and Sargassum fusiforme polysaccharide fermentation product includes: activating and culturing Lactobacillus in MRS medium at 30 - 37 °C for 18 - 24 h, inoculating it into the fermentation medium at 5 - 10% and fermenting at 30 - 37 °C for 24 - 48 h, then subjecting it to homogenization and crushing, centrifuging to remove residues, and drying to obtain the fermentation product; Among them, the fermentation medium is: 10 - 20 g / L glucose, 5 - 10 g / L yeast powder, 10 - 20 g / L soybean powder, 2 - 5 g / L seaweed powder, 0.5 - 5 g / L phycobiliprotein, 0.5 - 5 g / L Sargassum fusiforme polysaccharide, and the balance is deionized water.

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