Preparation method of sargassum fusiforme extract
Through macroporous resin adsorption and silica gel column purification technology, combined with alcohol precipitation and ultrafiltration technology, the problems of low extraction and recovery of active ingredients in yam sausage are solved, and the efficient and high-purity extraction effect is achieved, which is suitable for large-scale production.
Patent Information
- Application Number
- CN202510256906.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-05
- Publication Date
- 2025-06-06
AI Technical Summary
The prior art When extracting fucoxanthin, fucose gum and brown algae polyphenols from yam, the recovery rate is low, the purity is not high, and the industrial feasibility is low.
The macroporous resin adsorption and silica gel column purification technology are used, combined with alcohol precipitation and ultrafiltration technology, and fucoxanthin, fucose gum and brown algae polyphenols are extracted and purified in steps to improve recovery and purity.
It realizes efficient extraction and high-purity preparation of fucoxanthin, fucose gum and algae polyphenols, with a recovery rate of more than 90%, simplifies the process flow and is suitable for large-scale production.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of extraction and separation of Sargassum fusiformis, and specifically relates to a preparation method of a Sargassum fusiformis extract. Background Art
[0002] Sargassum fusiforme belongs to the genus Sargassum of the family Sargassum of the phylum Phaeophyceae, also known as antler weed and sea barley. It is rich in fucoxanthin, brown algae polyphenols and brown algae polysaccharides.
[0003] Fucoxanthin is a xanthophyll pigment unique to brown algae. It is chemically unstable and has strong antibacterial, weight loss, anti-tumor activity, blood sugar regulation and other physiological functions. It can be used as a food additive, feed colorant, medicine, health care products, and skin care and beauty products. However, the purity of fucoxanthin products on the market is only 0.5-5%.
[0004] Fucoidan is a type of polysaccharide extracted from brown algae, and Sargassum fusiformis polysaccharide is a specific type of fucoidan. Sargassum fusiformis polysaccharide is a water-soluble polysaccharide extracted from Sargassum fusiformis, which accounts for 48.28-63.73% of the dry weight of Sargassum fusiformis. The main components of Sargassum fusiformis polysaccharide are alginic acid, fucoidan and brown algae starch. Among them, fucoidan is an important active ingredient of Sargassum fusiformis polysaccharide, and its main components include fucose (more than 60%) and sulfate (10-40%).
[0005] The molecular structure of brown algae polyphenols is complex, mainly composed of phloroglucinol units to form polyhydroxy compounds. Its unique chemical structure gives it a variety of biological activities. From antioxidant and antibacterial to anti-inflammatory and anti-tumor, brown algae polyphenols show great potential in the fields of food, medicine and agriculture.
[0006] Patent CN105037300A discloses a method for comprehensive extraction of fucoxanthin and brown algae polyphenols from Sargassum. This method can prepare fucoxanthin with a purity higher than 75% and brown algae polyphenols with a purity of about 10% by extracting fucoxanthin through the selection of solvents. However, this method uses a large number of organic reagents for extraction, and the recovery rate of this method is low. In addition, because this method consumes a large amount of solvent, produces a lot of waste, and is prone to solvent residue, its industrial feasibility is low. Summary of the invention
[0007] In order to overcome the above technical problems, the present invention provides a method for preparing a Sargassum fusiformis extract. The preparation method of the present invention can simultaneously extract fucoxanthin, fucoidan and brown algae polyphenols, and the recovery rate of these three active ingredients and the product purity are all high.
[0008] The present invention solves the above technical problems through the following technical solutions.
[0009] The present invention discloses a method for preparing a Sargassum fusiformis extract, comprising the following steps:
[0010] S1. extracting the dried Sargassum fusiformis powder to obtain an extract A and a residue;
[0011] S2. The extract A is concentrated and precipitated with alcohol to obtain a precipitate A and a supernatant A, respectively;
[0012] S2.1. Dissolve the precipitate A and pass it through a macroporous resin and collect the effluent;
[0013] S2.2. The effluent is concentrated and treated to obtain the fucoxanthin product;
[0014] S3. The residue is subjected to water extraction, concentration, and alcohol precipitation to obtain a precipitate C and a supernatant B, respectively;
[0015] S3.1. Dissolve the precipitate C in water, remove impurities, and collect the precipitate D after alcohol precipitation;
[0016] S3.2. Dissolve the precipitate D in water and then perform ultrafiltration, and concentrate and dry the ultrafiltration interception liquid to obtain the fucoidan product;
[0017] S4. The supernatant A and the supernatant B are combined and concentrated, and then passed through a macroporous resin, and the effluent is concentrated and dried to obtain the brown algae polyphenol product.
[0018] In S1, the dried Sargassum fusiformis powder is obtained by grinding dried Sargassum fusiformis and then passing it through a 10-40 mesh sieve.
[0019] In S1, the content of fucoxanthin in the dry powder of Sargassum fusiformis is 0.18-0.21%, the content of brown algae polyphenols is 1.81-1.92%, and the content of brown algae polysaccharide is 48-52%; for example, the content of fucoxanthin in the dry powder of Sargassum fusiformis is 0.21%, the content of brown algae polyphenols is 1.86%, and the content of brown algae polysaccharide is 51.29%.
[0020] The ethanol of different concentrations in the present invention is all an ethanol-water system.
[0021] In S1, the extraction solvent is ethanol with a concentration of ≥95%; the material-liquid ratio of the extraction is 1:20-40 g / mL.
[0022] In S1, the extraction method is extraction tank extraction or continuous countercurrent extraction; the extraction process needs to be protected from light.
[0023] In S1, the extraction temperature is ≤50°C, the extraction time is 2 to 3 hours, and the extraction times are 1 to 2 times.
[0024] In S1, the extraction further requires the addition of an antioxidant; wherein the antioxidant is vitamin C or sodium sulfite; and the antioxidant accounts for 0.5-2% of the mass of the Sargassum fusiformis dry powder.
[0025] In S2, the concentration is to 40-50% of the original volume.
[0026] In S2, the solvent of the alcohol precipitation is 50-60% ethanol solution; the temperature of the alcohol precipitation is 4-10° C.; the operation of the alcohol precipitation is to collect the precipitate A and the supernatant A respectively after standing for 6-8 hours.
[0027] In S2.1, the solution obtained by dissolving the precipitate A in 95-100% ethanol passes through a macroporous resin; the macroporous resin is a non-polar macroporous resin or a weakly polar macroporous resin, such as D101 macroporous resin or AB-8 macroporous resin.
[0028] In S2.2, the concentration is to 40-50% of the original volume.
[0029] In S2.2, the treatment step is to collect the precipitate B after standing, and then dry the precipitate B to obtain the fucoxanthin product.
[0030] In S2.2, the standing temperature is 4 to 10° C., and the standing time is 8 to 12 hours.
[0031] In S2.2, the precipitate can also be dissolved in 95-100% ethanol and then passed through a silica gel column for further purification; the silica gel column is eluted with petroleum ether and ethyl acetate in sequence, and the effluent from the ethyl acetate section is collected.
[0032] In S2.2, the drying method is concentrated drying.
[0033] In S3, the solvent of the water extraction is water, and the solid-liquid ratio of the water extraction is 1:30-40 g / mL.
[0034] In S3, the water extraction temperature is 70-80°C, the water extraction time is 2-3 hours, and the water extraction is performed 1-3 times.
[0035] In S3, the water extraction is followed by centrifugation, filtration and merging.
[0036] In S3, the concentration is performed until the solid content is 10-15%.
[0037] In S3, the solvent for the alcohol precipitation is a 60-70% ethanol solution.
[0038] In S3, the temperature of the alcohol precipitation is 10-20° C., and the standing time of the alcohol precipitation is 8-12 hours.
[0039] In S3.1, the impurity removal method is precipitation method, and the impurity removal precipitant CaCl 2 ;
[0040] Wherein, the mass of the precipitant added is 2-5% of the mass of the precipitate C in parts by mass.
[0041] In S3.1, the standing time of the precipitation method for impurity removal is 2 to 4 hours, and after the precipitation method for impurity removal, the supernatant is collected and the precipitate is removed.
[0042] In S3.1, the solvent for the alcohol precipitation is a 65-75% ethanol solution; and the time for the alcohol precipitation is 8-12 hours.
[0043] In S3.2, the molecular weight cut-off of the ultrafiltration is 5 to 10 kDa.
[0044] In S4, the concentration is performed until the alcohol content is 10-15%.
[0045] In S4, the macroporous resin is a non-polar macroporous resin or a weakly polar macroporous resin, such as D101 macroporous resin or AB-8 macroporous resin.
[0046] In S4, the macroporous resin is eluted with water and 50-70% ethanol solution respectively, and the effluent of the 50-70% ethanol solution section is collected.
[0047] In the present invention, the purity of fucoxanthin in the fucoxanthin product is 98-99%, and the recovery rate of fucoxanthin in the fucoxanthin product is greater than 90%.
[0048] In the present invention, the content of fucose in the fucoidan product is greater than 25%, preferably 28.45% to 29.85%.
[0049] In the present invention, the sulfate content in the fucoidan product is greater than 30.2%, preferably 30.2-31.2%, such as 30.24%, 31.05%, 30.28%.
[0050] The purity of the brown algae polyphenol in the brown algae polyphenol product is greater than 56%, and the recovery rate of the brown algae polyphenol in the brown algae polyphenol product is greater than 90%.
[0051] On the basis of being in accordance with the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present invention.
[0052] Compared with the prior art, the present invention has the following beneficial effects:
[0053] 1. The present invention adopts macroporous resin adsorption and silica gel column purification technology to effectively remove impurities, obtain a fucoxanthin product with a purity of >70%, and a fucoxanthin recovery rate of >90%; in some preferred embodiments, the purity of the fucoxanthin product can reach 98-99%. At the same time, ultrafiltration technology is used to remove salt and some impurities, retain the biologically active components of fucoidan, and further purify through alcohol precipitation to obtain a fucose product with a fucose content of >25%; in some preferred embodiments, the fucose content in the fucoidan product can reach 28.45%-29.85%. In addition, with the adsorption and elution of macroporous resin, a brown algae polyphenol product with a purity of >56% is separated, and the recovery rate of brown algae polyphenol is >90%.
[0054] 2. During the extraction process, by selecting appropriate solvents and their concentrations, efficient extraction of the three active ingredients, fucoxanthin, fucoidan and brown algae polyphenols, can be achieved without the need for complex extraction and crystallization steps using multiple organic solvents, thereby simplifying the extraction process while ensuring high recovery rate and high purity.
[0055] 3. The separation process of the present invention is simple and easy to operate, suitable for large-scale production, high in production efficiency and less in pollution. In the industrial production process, the cost is low and has significant economic and environmental benefits. DETAILED DESCRIPTION
[0056] In order to facilitate the understanding of the present invention, the present invention will be described more comprehensively and carefully in combination with preferred embodiments below, but the protection scope of the present invention is not limited to the following specific embodiments.
[0057] Unless otherwise defined, all professional terms used below have the same meanings as those generally understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention.
[0058] After the raw material of Sargassum fusiformis was crushed, the content of fucoxanthin was tested to be 0.21%, the content of brown algae polyphenol was 1.86%, and the content of brown algae polysaccharide was 51.29%.
[0059] The determination of brown algae polyphenols in the following examples and comparative examples refers to GB 5009.238.
[0060] The determination of fucoxanthin refers to T / CAIAS 001-2021.
[0061] The determination of fucoidan refers to T / GXAF 0013-2023.
[0062] Sulfate determination steps: After dissolving the product, pass it through an ion chromatography column. The chromatographic column uses an anion exchange column (such as AS11-HC, 250mm×4mm) filled with ethylvinylbenzene-divinylbenzene polymer resin with quaternary ammonium as the functional group. The guard column uses an anion exchange column with the same filler (such as AG 11-HC, 50mm×4mm). The eluent is 20mmol / L ammonia oxidation solution (generated by an automatic eluent generator). The sulfate content is obtained by comparison with the standard curve.
[0063] Embodiment 1 (small test)
[0064] The dried Sargassum fusiformis was crushed and passed through a 40-mesh sieve to obtain 200 g of Sargassum fusiformis dry powder.
[0065] S1. The dried powder of Sargassum fusiformis was extracted with 95% ethanol in a light-proof extraction tank with a solid-liquid ratio of 1:40 g / mL, and 1 g of vitamin C (prepared into a 0.1 g / mL aqueous solution) as an antioxidant was added; the extraction was performed at 50°C for 2 h; after the extraction, extract A and residue were obtained respectively.
[0066] S2. After the extract A is concentrated to 40% of the original volume, water is added to dilute it to an ethanol concentration of 50%; after standing at 4°C for 8 hours, the precipitate A and the supernatant A are collected by filtration.
[0067] S2.1. Dissolve the precipitate A in 95% ethanol and pass the solution through D101 macroporous resin, and collect the effluent.
[0068] S2.2. The effluent was concentrated to 40% of the original volume and allowed to stand at 4°C for 8 h before collecting the precipitate B. The precipitate B was vacuum dried under light-proof conditions to obtain 0.53 g of fucoxanthin product. The purity of the fucoxanthin in the fucoxanthin product was found to be 71.23% and the recovery rate of the fucoxanthin was 90.02%.
[0069] S3. The residue was extracted with water, with a solid-liquid ratio of 1:30, an extraction temperature of 70°C, and an extraction time of 2h. After one extraction, the solid impurities were removed by centrifugation, and then concentrated to a solid content of 10%; then the ethanol concentration was adjusted to 60% (adjusted using 95% ethanol solution), placed at 10°C for alcohol precipitation for 8h, and the precipitate C and supernatant B were collected separately.
[0070] S3.1 Dissolve precipitate C in water and add CaCl 2 (The added mass is 5% of the mass of precipitate C) solution until no new precipitate appears, remove the precipitate; then adjust (using 95% ethanol solution) the ethanol concentration to 65%, precipitate for 8 hours, and collect the precipitate D.
[0071] S3.2. The precipitate D was washed with 90% ethanol and then dissolved with pure water. After centrifugation to remove solid impurities, ultrafiltration was performed. The ultrafiltration retention molecular weight was 5-10 kDa. The collected ultrafiltration retentate was concentrated and dried to obtain 8.09 g of fucoidan product. The fucose content in the fucoidan product was found to be 25.87% and the sulfate content was 30.28%.
[0072] S4. Supernatant A and supernatant B are combined and concentrated to an alcohol content of 10%, passed through D101 macroporous resin, and eluted with 1.5BV of pure water and 2BV of 50% ethanol solution in sequence, and the effluent from the 50% ethanol solution section is collected; the effluent is concentrated and dried to obtain 5.94g of brown algae polyphenol product. The purity of brown algae polyphenol in the brown algae polyphenol product is 56.38% and the recovery rate of brown algae polyphenol is 90.03%.
[0073] Example 2
[0074] This example explores the effect of ethanol concentration on extraction during S2 alcohol precipitation.
[0075] The difference between this embodiment and embodiment 1 is that:
[0076] The ethanol concentration and fucoxanthin recovery rate of the alcohol precipitation in S2 are shown in Table 1.
[0077] Table 1
[0078] Ethanol concentration (%) 60 65 70 Fucoxanthin product purity (%) 72.11 68.24 65.19 Fucoxanthin recovery rate (%) 90.52 88.24 85.16
[0079] Example 3 (pilot)
[0080] The dried Sargassum fusiformis was crushed and passed through a 40-mesh sieve to obtain 5000 g of Sargassum fusiformis dry powder.
[0081] S1. The dried powder of Sargassum fusiformis was extracted with 100% ethanol in a light-proof extraction tank with a solid-liquid ratio of 1:20 g / mL, and 100 g of vitamin C (prepared into a 0.2 g / mL aqueous solution) as an antioxidant was added; the extraction was performed at 45°C for 3 hours, for a total of two extractions, and after the extractions, extract A and residue were obtained respectively.
[0082] S2. After the extract A is concentrated to 50% of the original volume, water is added to dilute it to an ethanol concentration of 60%; after placing it at 8°C for 6 hours, the precipitate A and the supernatant A are collected by filtration.
[0083] S2.1. The solution of precipitate A dissolved in 100% ethanol (to remove insoluble impurities) was passed through AB-8 macroporous resin and the effluent was collected.
[0084] S2.2. The effluent was concentrated to 50% of the original volume, and the precipitate B was collected after standing at 8°C for 8 hours; the precipitate B was passed through a silica gel column and then vacuum dried under light-proof conditions to obtain 9.64 g of fucoxanthin product. The purity of fucoxanthin in the fucoxanthin product was 98.5% and the recovery rate of fucoxanthin was 90.20% after testing;
[0085] The precipitate B is dissolved in 100% ethanol and then passed through a silica gel column, and then eluted with petroleum ether and ethyl acetate in sequence, and the effluent from the ethyl acetate section is collected and then vacuum dried.
[0086] S3. The residue was extracted with water, with a solid-liquid ratio of 1:40, an extraction temperature of 80°C, and an extraction time of 3 hours. After two extractions, the mixture was centrifuged and concentrated to a solid content of 15%. The ethanol concentration was then adjusted to 70% (adjusted using 95% ethanol solution), placed at 15°C for alcohol precipitation for 10 hours, and the precipitate C and supernatant B were collected separately.
[0087] S3.1. Dissolve precipitate C in water and add CaCl 2 (The added mass is 4% of the mass of precipitate C) solution until no new precipitate appears, remove the precipitate; then adjust (using 100% ethanol solution) the ethanol concentration to 75%, precipitate for 12 hours, and collect the precipitate D.
[0088] S3.2. The precipitate D was washed with 90% ethanol and then dissolved with pure water. After centrifugation to remove solid impurities, ultrafiltration was performed. The ultrafiltration retention molecular weight was 5-10 kDa. The collected ultrafiltration retentate was concentrated and dried to obtain 202.4 g of fucoidan product. The fucose content in the fucoidan product was found to be 29.85% and the sulfate content was 31.05%.
[0089] S4 supernatant A and supernatant B are combined and concentrated to an alcohol content of 15%, passed through AB-8 macroporous resin, and eluted with 2BV pure water and 2.5BV 60% ethanol solution in sequence, and the 60% ethanol solution segment effluent is collected; the effluent is concentrated and dried to obtain 145.7g of brown algae polyphenol product. After testing, the purity of brown algae polyphenol is 58.21% and the recovery rate of brown algae polyphenol is 91.20%.
[0090] Embodiment 4 (trial production)
[0091] The dried Sargassum fusiformis was crushed and passed through a 40-mesh sieve to obtain 100 kg of Sargassum fusiformis dry powder.
[0092] S1. The dried powder of Sargassum fusiformis was extracted with 100% ethanol in the dark with a solid-liquid ratio of 1:30 g / mL, and 500 g of vitamin C (prepared into a 0.2 g / mL aqueous solution) as an antioxidant was added; countercurrent extraction was performed continuously at 45°C for 3 hours, and after extraction, extract A and residue were obtained respectively.
[0093] S2. After the extract A is concentrated to 50% of the original volume, water is added to dilute it to an ethanol concentration of 50%; after placing it at 10°C for 6 hours, the precipitate A and the supernatant A are collected by filtration.
[0094] S2.1. The solution of precipitate A dissolved in 95% ethanol (to remove insoluble impurities) is passed through D101 macroporous resin and the effluent is collected.
[0095] S2.2. The effluent was concentrated to 50% of the original volume, and the precipitate B was collected after standing at 8°C for 8 hours; the precipitate B was passed through a silica gel column and then vacuum dried under light-proof conditions to obtain 192.6 g of fucoxanthin product. The purity of fucoxanthin in the fucoxanthin product was tested to be 99.0%, and the recovery rate of fucoxanthin was 90.80%.
[0096] The precipitate B is dissolved with 95% ethanol and then passed through a silica gel column, and eluted with petroleum ether and ethyl acetate in sequence, and the effluent from the ethyl acetate section is collected and then vacuum dried.
[0097] S3. The residue was subjected to continuous countercurrent extraction with water, with a solid-liquid ratio of 1:30, an extraction temperature of 70°C, and an extraction time of 3 hours. After two extractions, the mixture was centrifuged to remove impurities and then concentrated to a solid content of 10%. The ethanol concentration was then adjusted to 60% (adjusted using 95% ethanol solution), placed at 20°C for alcohol precipitation for 12 hours, and the precipitate C and supernatant B were collected separately.
[0098] S3.1. Dissolve precipitate C in water and add CaCl 2 (The added mass is 5% of the mass of precipitate C) solution until no new precipitate appears; then adjust (using 100% ethanol solution) the ethanol concentration to 75%, precipitate for 12 hours, and collect precipitate D.
[0099] S3.2. The precipitate D was washed with 90% ethanol and then dissolved with pure water. The solid impurities were removed by centrifugation and then ultrafiltration was performed. The precipitate D was ultrafiltered with an ultrafiltration cutoff molecular weight of 5 to 10 kDa. The collected ultrafiltration retentate was concentrated and dried to obtain 8.09 kg of fucoidan product. The fucose content in the fucoidan product was found to be 28.45% and the sulfate content was 30.24%.
[0100] S4 supernatant A and supernatant B are combined and concentrated to an alcohol content of 15%, passed through D101 macroporous resin, eluted with 2BV pure water to remove impurities, and then eluted with 2.5BV 70% ethanol solution, and the effluent from the 70% ethanol solution section was collected; the effluent was concentrated and dried to obtain 2.94kg of brown algae polyphenol product. After testing, the purity of brown algae polyphenol in the brown algae polyphenol product was 57.18%, and the recovery rate of brown algae polyphenol was 90.38%.
[0101] Comparative Example 1
[0102] The difference between this comparative example and Example 1 is:
[0103] In step S1., no vitamins were added and the extraction time was 2 h.
[0104] The standing time in step S2.2. is 12 h.
[0105] 0.49 g of fucoxanthin product was obtained, the purity of fucoxanthin in the fucoxanthin product was 68.54%, and the recovery rate of fucoxanthin was 80.14%.
[0106] Comparative Example 2
[0107] The difference between this comparative example and Example 1 is:
[0108] The S1 extraction process was not protected from light, and the purity of fucoxanthin in the fucoxanthin product was 62.15%, and the recovery rate of fucoxanthin was 81.25%.
[0109] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods. The specific embodiments described above further describe the purpose, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing a Sargassum fusiformis extract, characterized in that: The following steps are involved: S1. extracting the dried Sargassum fusiformis powder to obtain an extract A and a residue; S2. The extract A is concentrated and precipitated with alcohol to obtain a precipitate A and a supernatant A, respectively; S2.
1. Dissolve the precipitate A and pass it through a macroporous resin and collect the effluent; S2.
2. The effluent is concentrated and treated to obtain the fucoxanthin product; S3. The residue is subjected to water extraction, concentration, and alcohol precipitation to obtain a precipitate C and a supernatant B, respectively; S3.
1. Dissolve the precipitate C in water, remove impurities, and collect the precipitate D after alcohol precipitation; S3.
2. Dissolve the precipitate D in water and then perform ultrafiltration, and concentrate and dry the ultrafiltration interception liquid to obtain the fucoidan product; S4. The supernatant A and the supernatant B are combined and concentrated, and then passed through a macroporous resin, and the effluent is concentrated and dried to obtain the brown algae polyphenol product.
2. The method for preparing the Sargassum fusiformis extract according to claim 1, wherein Satisfy at least one of the following conditions ①~②: ① The dried Sargassum fusiformis powder is obtained by grinding dried Sargassum fusiformis and then passing it through a 10-40 mesh sieve; ② The content of fucoxanthin in the dried Sargassum fusiformis powder is 0.18-0.21%, the content of brown algae polyphenol is 1.81-1.92%, and the content of brown algae polysaccharide is 48-52%.
3. The method for preparing the Sargassum fusiformis extract according to claim 1, characterized in that: Satisfy at least one of the following conditions ① to ⑥: ① In S1, the extraction solvent is ethanol with a concentration of ≥ 95%; ② In S1, the solid-liquid ratio of the extraction is 1:20-40 g / mL; ③ In S1, the extraction method is extraction tank extraction or continuous countercurrent extraction; ④ In S1, the extraction process needs to be protected from light; ⑤ In S1, the extraction temperature is ≤50°C and the extraction time is 2 to 3 hours; ⑥ In S1, the extraction further requires the addition of an antioxidant; wherein the antioxidant is vitamin C or sodium sulfite; the antioxidant accounts for 0.5 to 2% of the mass of the Sargassum fusiformis dry powder.
4. The method for preparing the Sargassum fusiformis extract according to claim 1, characterized in that: Satisfy at least one of the following conditions ①~②: ① In S2, the concentration is to 40-50% of the original volume; ② In S2, the solvent of the alcohol precipitation is 50-60% ethanol solution; the temperature of the alcohol precipitation is 4-10° C.; the operation of the alcohol precipitation is to collect the precipitate A and the supernatant A respectively after standing for 6-8 hours.
5. The method for preparing the Sargassum fusiformis extract according to claim 1, characterized in that: Satisfy at least one of the following conditions ① to ③: ① In S2.1, the solution obtained by dissolving the precipitate A in 95-100% ethanol passes through a macroporous resin; wherein the macroporous resin is a non-polar macroporous resin or a weakly polar macroporous resin; ② In S2.2, the concentration is to 40-50% of the original volume; ③ In S2.2, the treatment step is to collect the precipitate B after standing, and then dry the precipitate B to obtain the fucoxanthin product; the standing temperature is 4 to 10°C, and the standing time is 8 to 12 hours.
6. The method for preparing the Sargassum fusiformis extract according to claim 1, characterized in that: Satisfy at least one of the following conditions ① to ⑥: ① In S3, the solid-liquid ratio of the water extraction is 1:30-40 g / mL; ② In S3, the water extraction temperature is 70-80° C., and the water extraction time is 2-3 hours; ③ In S3, the water extraction is further followed by centrifugation, filtration and merging; ④ In S3, the concentration is to a solid content of 10-15%; ⑤ In S3, the solvent of the alcohol precipitation is 60-70% ethanol solution; ⑥ In S3, the temperature of the alcohol precipitation is 10-20° C., and the standing time of the alcohol precipitation is 8-12 hours.
7. The method for preparing the Sargassum fusiformis extract according to claim 1, characterized in that: Satisfy at least one of the following conditions ① to ③: ① In S3.1, the impurity removal method is precipitation removal, and the impurity removal precipitant is CaCl2; Wherein, the mass of the precipitant added is 2-5% of the mass of the precipitate C in parts by mass; ② In S3.1, the standing time of the precipitation method is 2 to 4 hours, and after the precipitation method is used for impurity removal, the supernatant is collected and the precipitate is removed; ③ In S3.1, the solvent of the alcohol precipitation is 65-75% ethanol solution; the time of the alcohol precipitation is 8-12 hours.
8. The method for preparing the Sargassum fusiformis extract according to claim 1, characterized in that: In S3.2, the molecular weight cut-off of the ultrafiltration is 5 to 10 kDa.
9. The method for preparing the Sargassum fusiformis extract according to claim 1, characterized in that: Satisfy at least one of the following conditions ① to ③: ① In S4, the concentration is performed to an alcohol content of 10 to 15%; ② In S4, the macroporous resin is a non-polar macroporous resin or a weakly polar macroporous resin; ③ In S4, the macroporous resin is eluted with water and 50-70% ethanol solution respectively, and the effluent of the 50-70% ethanol solution section is collected.
10. The method for preparing the Sargassum fusiformis extract according to any one of claims 1 to 9, characterized in that: Satisfy at least one of the following conditions ① to ③: ① The purity of fucoxanthin in the fucoxanthin product is 98-99%, and the recovery rate of fucoxanthin in the fucoxanthin product is >90%; ② The content of fucose in the fucoidan product is greater than 25%; ③ The purity of the brown algae polyphenols in the brown algae polyphenol product is greater than 56%, and the recovery rate of the brown algae polyphenols in the brown algae polyphenols is greater than 90%.
Citation Information
Patent Citations
Method for comprehensively extracting fucoxanthin and brown alga polyphenol from gulfweed
CN105037300A