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CN105193863B - A kind of preparation method of high-purity seeweed polyphenol - Google Patents

A kind of preparation method of high-purity seeweed polyphenol Download PDF

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CN105193863B
CN105193863B CN201510648035.0A CN201510648035A CN105193863B CN 105193863 B CN105193863 B CN 105193863B CN 201510648035 A CN201510648035 A CN 201510648035A CN 105193863 B CN105193863 B CN 105193863B
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CN105193863A (en
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刘翼翔
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Xiamen Aiyi Snack Research Institute Co ltd
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Abstract

本发明公开了一种高纯度海藻多酚的制备方法,包括海藻多糖与海藻渣的分离、海藻渣的酶解破壁、海藻多酚的高效提取、海藻多酚的分离纯化、高纯度海藻多酚的获得等工艺步骤,实现了海藻多糖、海藻多酚、海藻渣的全藻综合利用。

The invention discloses a preparation method of high-purity seaweed polyphenols, which comprises separation of seaweed polysaccharides and seaweed residues, enzymatic hydrolysis of seaweed residues, high-efficiency extraction of seaweed polyphenols, separation and purification of seaweed polyphenols, high-purity seaweed polyphenols The process steps such as the acquisition of phenol have realized the comprehensive utilization of the whole algae of seaweed polysaccharides, seaweed polyphenols and seaweed residue.

Description

一种高纯度海藻多酚的制备方法A kind of preparation method of high-purity seaweed polyphenol

技术领域technical field

本发明涉及海藻多酚的技术领域,尤其涉及一种高纯度海藻多酚的制备方法。The invention relates to the technical field of seaweed polyphenols, in particular to a preparation method of high-purity seaweed polyphenols.

背景技术Background technique

海藻是海洋植物多酚的主要来源,其结构与陆源植物多酚存在很大不同:陆源植物多酚是由没食子酸和糅花酸衍生而来;海藻多酚则是间苯三酚的衍生物。研究显示,海藻多酚在抗氧化、改善代谢综合症、防治退行性疾病等方面有特效,且安全无毒。因此,欧美国家已相继投入巨资实施海藻多酚的开发应用。高纯度海藻多酚具有生物活性强、医用价值高、稳定性好等优势,是生物医药领域迫切需求的产品。Seaweed is the main source of marine plant polyphenols, and its structure is quite different from that of terrestrial plant polyphenols: terrestrial plant polyphenols are derived from gallic acid and halide acid; seaweed polyphenols are derivatives of phloroglucinol . Studies have shown that seaweed polyphenols have special effects in anti-oxidation, improving metabolic syndrome, and preventing degenerative diseases, and are safe and non-toxic. Therefore, European and American countries have invested heavily in the development and application of seaweed polyphenols. High-purity seaweed polyphenols have the advantages of strong biological activity, high medical value, and good stability, and are urgently needed products in the field of biomedicine.

然而,由于海藻多酚存在于海藻细胞内部的藻泡中,被藻胶、纤维素等深度包埋,常规萃取技术很难获得高产率,生产成本极高,纯度较低。例如,中国发明专利申请CN102579508A《一种羊栖菜褐藻多酚的制备方法》,公开以羊栖菜为原料,采用甲醇加热提取(40℃),然后采用不同溶剂萃取及超滤截留手段制备得到褐藻多酚;中国发明专利申请CN102397300A《一种褐藻多酚的提取方法》,公开以新鲜海带、鼠尾藻、海黍子为原料,采用机溶剂提取、大孔树脂纯化制备得到3种褐藻多酚,其产率分别为0.3‰、2.5‰、3‰;中国发明专利申请CN103610704A《一种褐藻多酚的提取方法》,公开以新鲜马尾藻属褐藻或海带为原料,破碎后采用有机溶剂在热水浴中浸提,经大孔树脂纯化、洗脱、浓缩、冷冻干燥后得到褐藻多酚提取物,产率为2.5‰;中国发明专利申请CN104382951A《一种海藻多酚的提取方法》,公开以蛋白核小球藻、裸藻、盐藻三种藻类为原料,以乙醇为溶剂,采用微波联合提取技术,提取液过滤后经冷冻干燥得到3种海藻的多酚提取物;中国发明专利授权CN102935093B《一种海藻多酚的提取方法》,公开以40目的海藻粉为原料,采用微波辅助水提法进行提取,然后经大孔树脂纯化得到纯度75%左右的多酚提取物;中国发明专利授权CN102166230B《微波辅助海藻多酚的方法》,公开以海藻粉为原料,以醇-丙酮-水混合溶剂,结合微波技术提取海藻多酚,经过滤、冷冻干燥得到海藻多酚粗提物,提取率可达2.26%。上述制备海藻多酚的方法缺乏对褐藻胶等主要成分的综合利用,资源浪费严重;同时上述制备海藻多酚的工艺技术还存在以下问题:1)分离效果差,纯度低。海藻多酚易与海藻胶、蛋白以非共价键的形式形成复合物,在后续的纯化过程很难将其分离,导致海藻多酚的回收率低;此外,提取的海藻多酚中还含有大量脂溶性色素,传统柱层析技术无法实现有效分离,导致产品的纯度低。2)结构破坏大,活性低。海藻多酚极不稳定,易氧化,加工过程中的高温、碱性pH值、氧等均会破坏其生物活性。虽然微波技术、超声波辅助萃取技术能够提高海藻洋多酚的得率,但提取过程会产生高温,加上缺乏有效保护措施,在氧的作用下加速了海洋多酚的氧化,导致活性丧失。3)生产工艺复杂,成本高。目前用于加工海藻多酚的工艺包括粉碎、提取、离心、过滤、上柱、洗脱、树脂再生、多次浓缩、干燥等多道工序;常规柱层析纯化海藻多酚还必须配备恒流泵、玻璃柱、收集装置等设备,导致生产时间长,设备要求高,限制了产业化发展。这是导致海藻多酚产业化应用的关键技术瓶颈。However, because seaweed polyphenols exist in algal vesicles inside seaweed cells and are deeply embedded by alginate, cellulose, etc., conventional extraction techniques are difficult to obtain high yields, and the production cost is extremely high and the purity is low. For example, the Chinese invention patent application CN102579508A "A Preparation Method of Fujiki Brown Algae Polyphenols" discloses that hijiki is used as raw material, heated and extracted with methanol (40°C), and then prepared by different solvent extraction and ultrafiltration interception means. Brown algae polyphenols; Chinese invention patent application CN102397300A "Extraction method of brown algae polyphenols", which discloses that fresh kelp, sage, sea broomcorns are used as raw materials, and three kinds of brown algae polyphenols are obtained by extracting with organic solvents and purifying macroporous resins. Phenols, whose yields are respectively 0.3‰, 2.5‰, and 3‰; Chinese invention patent application CN103610704A "A Method for Extracting Brown Algae Polyphenols" discloses that fresh Sargassum brown algae or kelp are used as raw materials. Extraction in a hot water bath, purification, elution, concentration, and freeze-drying of macroporous resins to obtain brown algae polyphenol extracts, with a yield of 2.5‰; Chinese invention patent application CN104382951A "A Method for Extracting Seaweed Polyphenols", It is disclosed that three kinds of algae, Chlorella pyrenoidosa, Euglena, and Salina, are used as raw materials, ethanol is used as a solvent, and microwave combined extraction technology is used. The extract is filtered and freeze-dried to obtain polyphenol extracts of three kinds of seaweeds; Chinese invention patent Authorized CN102935093B "A Method for Extracting Seaweed Polyphenols", which discloses that 40-mesh seaweed powder is used as raw material, extracted by microwave-assisted water extraction, and then purified by macroporous resin to obtain a polyphenol extract with a purity of about 75%. Invented in China Patent authorization CN102166230B "Microwave Assisted Seaweed Polyphenol Method" discloses that seaweed polyphenols are extracted by using seaweed powder as raw material, alcohol-acetone-water mixed solvent, combined with microwave technology, filtered and freeze-dried to obtain a crude seaweed polyphenol extract. The extraction rate can reach 2.26%. The above-mentioned method for preparing seaweed polyphenol lacks the comprehensive utilization of main components such as alginate, resulting in a serious waste of resources; meanwhile, the above-mentioned process for preparing seaweed polyphenol still has the following problems: 1) The separation effect is poor and the purity is low. Seaweed polyphenols are easy to form complexes with seaweed gum and protein in the form of non-covalent bonds, and it is difficult to separate them in the subsequent purification process, resulting in a low recovery rate of seaweed polyphenols; in addition, the extracted seaweed polyphenols also contain A large amount of fat-soluble pigments cannot be effectively separated by traditional column chromatography, resulting in low product purity. 2) The structure is greatly damaged and the activity is low. Seaweed polyphenols are extremely unstable and easily oxidized, and high temperature, alkaline pH, oxygen, etc. during processing will destroy their biological activity. Although microwave technology and ultrasonic-assisted extraction technology can improve the yield of marine polyphenols, the extraction process will generate high temperature, coupled with the lack of effective protection measures, the oxidation of marine polyphenols will be accelerated under the action of oxygen, resulting in the loss of activity. 3) The production process is complicated and the cost is high. The current process for processing seaweed polyphenols includes multiple processes such as crushing, extraction, centrifugation, filtration, column loading, elution, resin regeneration, multiple concentration, and drying; conventional column chromatography purification of seaweed polyphenols must also be equipped with a constant flow Pumps, glass columns, collection devices and other equipment lead to long production time and high equipment requirements, which limits the development of industrialization. This is the key technical bottleneck leading to the industrial application of seaweed polyphenols.

有鉴于此,本发明人研究和设计了一种高纯度海藻多酚的制备方法,本案由此产生。In view of this, the present inventor has researched and designed a method for preparing high-purity seaweed polyphenols, and this case arises from it.

发明内容Contents of the invention

本发明的目的在于提供一种高纯度海藻多酚的制备方法,包括海藻多糖与海藻渣的分离、海藻渣的酶解破壁、海藻多酚的高效提取、海藻多酚的分离纯化、高纯度海藻多酚的获得等工艺步骤,以实现海藻多糖、海藻多酚、海藻渣的全藻综合利用。The purpose of the present invention is to provide a method for preparing high-purity seaweed polyphenols, including the separation of seaweed polysaccharides and seaweed residues, enzymolysis of seaweed residues, efficient extraction of seaweed polyphenols, separation and purification of seaweed polyphenols, high-purity Process steps such as the acquisition of seaweed polyphenols to realize the comprehensive utilization of seaweed polysaccharides, seaweed polyphenols, and seaweed residues.

为了实现上述目的,本发明解决其技术问题所采取的技术方案是:In order to achieve the above object, the technical solution taken by the present invention to solve the technical problems is:

一种高纯度海藻多酚的制备方法,包括以下步骤:A preparation method of high-purity seaweed polyphenols, comprising the following steps:

步骤一、海藻多糖与海藻渣的分离:首先将含水量为20%的干海藻用自来水浸泡,漂洗除去泥沙杂质后用打浆机打浆;海藻浆送入搅拌机中,并按海藻浆:去离子水体积比为1:5加入去离子水,室温下以120转/min转速搅拌30分钟;海藻浆用低速离心机以1000转/min的转速离心5min,分别收集上清液和海藻渣;海藻渣按上述步骤及条件经搅拌机搅拌、离心机离心处理后,再次分别收集上清液和海藻渣;合并两次上清液,经喷雾干燥后得到海藻多糖;收集海藻渣,用于提取制备海藻多酚;Step 1. Separation of seaweed polysaccharides and seaweed residue: first soak the dried seaweed with a water content of 20% in tap water, rinse to remove sediment impurities, and beat with a beater; send the seaweed pulp into the mixer, and press the seaweed pulp: deionized The water volume ratio is 1:5, add deionized water, stir at room temperature at 120 rpm for 30 minutes; use a low-speed centrifuge to centrifuge the seaweed slurry at 1000 rpm for 5 minutes, and collect the supernatant and seaweed residue; After the slag is stirred by a mixer and centrifuged in a centrifuge according to the above steps and conditions, the supernatant and seaweed residue are collected separately again; the two supernatants are combined and spray-dried to obtain seaweed polysaccharide; the seaweed residue is collected for extraction and preparation of seaweed polyphenols;

步骤二、海藻渣的酶解破壁:将由纤维素酶与果胶酶按重量比1:1组成的复合酶按重量比为1:1000加入到所述海藻渣中,室温下水解5h,实现海藻细胞壁破壁;Step 2. Enzymatic hydrolysis of seaweed dregs: add a compound enzyme composed of cellulase and pectinase in a weight ratio of 1:1000 to the seaweed dregs, and hydrolyze for 5 hours at room temperature to achieve Algae cell wall breakdown;

步骤三、海藻多酚的高效提取:将海藻多酚保护剂溶解于去离子水中,然后与食品级无水乙醇按体积比为1:4混合,并按体积比加入醋酸,使醋酸终体积浓度为0.1%,混匀后为海藻多酚的提取液;所述提取液与海藻渣按体积/重量比为5:1进行混匀,室温下提取1.5h,以3000转/min的转速离心5min,分别收集上清液和海藻渣;海藻渣继续用所述提取液重复前述步骤进行二次提取,分别收集上清液和海藻渣;海藻渣经干燥后用于饲料添加剂原料;合并两次上清液,用于海藻多酚的分离纯化;Step 3. High-efficiency extraction of seaweed polyphenols: dissolve the seaweed polyphenol protective agent in deionized water, then mix it with food-grade absolute ethanol at a volume ratio of 1:4, and add acetic acid according to the volume ratio to make the final volume concentration of acetic acid 0.1%, after mixing, it is the extract of seaweed polyphenols; the extract and seaweed residue are mixed at a volume/weight ratio of 5:1, extracted at room temperature for 1.5h, and centrifuged at 3000 rpm for 5min , collect supernatant and seaweed residue respectively; seaweed residue continues to use the extract to repeat the above steps for secondary extraction, collect supernatant and seaweed residue respectively; seaweed residue is used as feed additive raw material after being dried; Serum, used for the separation and purification of seaweed polyphenols;

步骤四、海藻多酚的分离纯化:将步骤三制得的上清液倒入含有硅胶的吸附池进行静态吸附脱色2h,硅胶吸附的色素进一步用于制备岩藻黄质活性物质;然后采用减压浓缩法在40℃下将海藻多酚提取液浓缩至50%体积后,采用国产XDA-7大孔吸收树脂对海藻多酚进行固相萃取2h;将XDA-7大孔树脂用去离子水快速漂洗,除去糖、小肽杂质;然后将XDA-7大孔树脂用食品级无水乙醇浸泡0.5h,将吸附于大孔树脂上的海藻多酚洗脱并溶解于乙醇中,得到乙醇浸泡液;Step 4. Separation and purification of seaweed polyphenols: pour the supernatant obtained in step 3 into an adsorption pool containing silica gel for static adsorption and decolorization for 2 hours, and the pigment adsorbed by silica gel is further used to prepare fucoxanthin active substances; After the seaweed polyphenol extract was concentrated to 50% volume at 40°C by the pressure concentration method, the seaweed polyphenol was subjected to solid-phase extraction with domestic XDA-7 macroporous absorption resin for 2 hours; the XDA-7 macroporous resin was deionized water Rinse quickly to remove sugar and small peptide impurities; then soak the XDA-7 macroporous resin in food-grade anhydrous ethanol for 0.5h, elute the seaweed polyphenols adsorbed on the macroporous resin and dissolve them in ethanol to obtain ethanol-soaked liquid;

步骤五、海藻多酚的制备:将所述乙醇浸泡液在40℃下减压浓缩至干,在50℃下真空干燥2h,得到海藻多酚产品。Step 5, preparation of seaweed polyphenols: the ethanol soaking solution was concentrated to dryness under reduced pressure at 40° C., and vacuum-dried at 50° C. for 2 hours to obtain seaweed polyphenol products.

作为实施例的优选方式,所述海藻为海带、裙带菜、羊牺菜、海黍子、鼠尾藻和甘苔中的至少一种。As a preferred embodiment of the embodiment, the seaweed is at least one of kelp, wakame, sagittaria, sea sorghum, sagera, and licorice.

作为实施例的优选方式,所述步骤三的海藻多酚保护剂为维生素C或植酸或由维生素C与植酸组成的复合物。As a preferred embodiment of the embodiment, the seaweed polyphenol protective agent in the third step is vitamin C or phytic acid or a complex composed of vitamin C and phytic acid.

作为实施例的优选方式,所述步骤三的提取液中含有质量体积比为0.05-0.5%的维生素C。As a preferred mode of the embodiment, the extract in the third step contains vitamin C with a mass volume ratio of 0.05-0.5%.

作为实施例的优选方式,所述步骤三的提取液中含有体积比为0.01-0.1%的植酸。As a preferred mode of the embodiment, the extract in the third step contains 0.01-0.1% phytic acid by volume.

作为实施例的优选方式,所述步骤三的提取液中含有质量体积比为0.05-0.1%的维生素C及体积比为0.01-0.05%的植酸。As a preferred embodiment of the embodiment, the extract in step 3 contains vitamin C with a mass volume ratio of 0.05-0.1% and phytic acid with a volume ratio of 0.01-0.05%.

作为实施例的优选方式,所述海藻多酚产品为白色粉末;所述海藻多酚的提取率为1.5-6.5%;纯度为90-95%。As a preferred form of the embodiment, the seaweed polyphenol product is white powder; the extraction rate of the seaweed polyphenol is 1.5-6.5%; the purity is 90-95%.

本发明采用以上技术方案后,具有以下有益效果:After the present invention adopts the above technical scheme, it has the following beneficial effects:

1.本发明可实现海藻多糖、海藻多酚、岩藻黄质、海藻渣的全藻资源利用,是海藻加工业迫切需求的核心技术;1. The present invention can realize the utilization of whole algal resources of seaweed polysaccharides, seaweed polyphenols, fucoxanthin and seaweed residue, which is the core technology urgently needed by the seaweed processing industry;

2.本发明采用固相萃取技术实现海藻多酚的高效分离纯化,减少常规海藻多酚生产工艺中的过滤、柱层析纯化、浓缩等单元操作,简化工艺流程,缩短生产时间,提高了产品质量,产品纯度均≥90质量%;2. The present invention adopts solid-phase extraction technology to realize high-efficiency separation and purification of seaweed polyphenols, reduces unit operations such as filtration, column chromatography purification, and concentration in conventional seaweed polyphenol production processes, simplifies the process flow, shortens production time, and improves product quality. Quality, product purity ≥ 90% by mass;

3.本发明针对海藻多酚易氧化降解的特点,在提取过程中通过添加保护剂提高了海藻多酚的稳定性,从而提高了提取效率。3. The present invention aims at the characteristics that seaweed polyphenols are easy to oxidize and degrade, and improves the stability of seaweed polyphenols by adding a protective agent during the extraction process, thereby improving the extraction efficiency.

附图说明Description of drawings

图1为本发明的工艺流程图。Fig. 1 is a process flow diagram of the present invention.

具体实施方式Detailed ways

下面详细描述本发明的实施例,本发明的工艺流程图,如图1所示。通过参考附图描述的实施例是示例性的,旨在用于解释本发明,而不能理解为对本发明的限制。实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规产品。Embodiments of the present invention are described in detail below, and the process flow diagram of the present invention is shown in FIG. 1 . The embodiments described by referring to the figures are exemplary and are intended to explain the present invention and should not be construed as limiting the present invention. If no specific technique or condition is indicated in the examples, it shall be carried out according to the technique or condition described in the literature in this field or according to the product specification. The reagents or instruments used were not indicated by the manufacturer, and they were all commercially available conventional products.

以下实施例所用的复合酶为1:1(w/w)的果胶酶和纤维素酶复合酶;提取液中的保护剂为0.05质量%与0.01体积%植酸。The compound enzyme used in the following examples is a 1:1 (w/w) pectinase and cellulase compound enzyme; the protective agent in the extract is 0.05 mass % and 0.01 volume % phytic acid.

实施例1:海带制备高纯度海藻多酚Example 1: Preparation of high-purity seaweed polyphenols from kelp

(1)取含水量为20质量%干海带1kg,用自来水浸泡漂洗除去泥沙等杂质后用打浆机打浆,得到海藻浆0.6L;送入搅拌器中,并加入3L去离子水,温下以120转/min转速搅拌30min;海藻浆然后用低速离心机以1000转/min的转速离心5min,分别收集上清液和海藻渣;海藻渣按上述步骤及条件经搅拌机搅拌、离心机离心处理后,再次分别收集上清液和海藻渣。合并两次上清液,经喷雾干燥后得到海藻多糖;收集得到海藻渣342g,用于提取制备海藻多酚。(1) Get water content and be 20 mass % dry sea-tangle 1kg, after soaking and rinsing with tap water to remove impurities such as silt, beating with a beater to obtain 0.6L of seaweed slurry; send it into the agitator, and add 3L deionized water, under temperature Stir at a speed of 120 rpm for 30 minutes; then use a low-speed centrifuge to centrifuge the seaweed slurry at a speed of 1000 rpm for 5 minutes to collect the supernatant and seaweed residue; the seaweed residue is stirred by a mixer and centrifuged in a centrifuge according to the above steps and conditions Afterwards, the supernatant and seaweed residue were collected again. The two supernatants were combined and spray-dried to obtain seaweed polysaccharides; 342 g of seaweed residue was collected for extraction and preparation of seaweed polyphenols.

(2)取上述湿海带渣与1.71g复合酶混合均匀,室温下水解5h,实现海藻细胞壁破壁。(2) Mix the wet kelp slag with 1.71 g of compound enzyme evenly, and hydrolyze it at room temperature for 5 hours to break the cell wall of seaweed.

(3)将海藻多酚保护剂溶解于去离子水中,然后与食品级无水乙醇按体积比为1:4(v:v)混合,并按体积比加入醋酸,使醋酸终浓度为0.1%(v:v),混匀后为海藻多酚的提取液,提取液中含0.05质量%与0.01体积%植酸。1.71L提取液加入到上述酶解破壁的海藻渣中并混匀,室温下提取1.5h;然后以3000转/min的转速离心5min,分别收集上清液和海藻渣。海藻渣继续用上述提取液重复前述步骤进行二次提取,分别收集上清液和海藻渣。海藻渣经干燥后用于饲料添加剂原料;合并两次上清液3.2L,用于海藻多酚的分离纯化。(3) Dissolve the seaweed polyphenol protective agent in deionized water, then mix it with food-grade absolute ethanol in a volume ratio of 1:4 (v:v), and add acetic acid in a volume ratio to make the final concentration of acetic acid 0.1%. (v:v), after mixing, it is an extract of seaweed polyphenols, and the extract contains 0.05% by mass and 0.01% by volume of phytic acid. Add 1.71L of the extract to the above-mentioned enzymatically broken seaweed residue and mix well, extract at room temperature for 1.5h; then centrifuge at 3000 rpm for 5min, and collect the supernatant and seaweed residue respectively. Seaweed dregs continue to use the above extract to repeat the aforementioned steps for secondary extraction, and collect the supernatant and seaweed dregs respectively. Seaweed dregs were dried and used as raw materials for feed additives; 3.2 L of the two supernatants were combined for separation and purification of seaweed polyphenols.

(4)将上述上清液倒入装有硅胶的吸附池,使液面与硅胶齐平,进行静态吸附脱色2h,硅胶吸附的色素可进一步用于制备岩藻黄质等活性物质;然后采用减压浓缩法在40℃下将海藻多酚提取液浓缩至1.6L体积后,将浓缩液倒入装有国产XDA-7大孔吸收树脂的吸附池,使液面与大孔树脂齐平,对海藻多酚进行固相萃取2h;用滤网将大孔树脂捞出,用去离子水快速漂洗,除去糖、小肽等杂质;然后将大孔树脂放入装有食品级无水乙醇的解吸附池,使乙醇液面与大孔树脂齐平,浸泡0.5h,使吸附于大孔树脂上的海藻多酚洗脱并溶解于乙醇中。解吸附的大孔树脂经去离子水漂洗后再用于下一次海藻多酚的吸附;解吸附池中乙醇可多次反复使用,以达到富集海藻多酚的目的。(4) Pour the above-mentioned supernatant into an adsorption tank equipped with silica gel, make the liquid level flush with silica gel, carry out static adsorption decolorization for 2 hours, and the pigments adsorbed by silica gel can be further used to prepare active substances such as fucoxanthin; then use The reduced-pressure concentration method concentrates the seaweed polyphenol extract to a volume of 1.6L at 40°C, and then pours the concentrated solution into an adsorption pool equipped with domestic XDA-7 macroporous absorbent resin so that the liquid level is flush with the macroporous resin. Carry out solid-phase extraction of seaweed polyphenols for 2 hours; remove the macroporous resin with a filter, rinse quickly with deionized water to remove impurities such as sugar and small peptides; then put the macroporous resin into a container filled with food-grade absolute ethanol Desorption tank, make the ethanol liquid level flush with the macroporous resin, soak for 0.5h, so that the seaweed polyphenols adsorbed on the macroporous resin are eluted and dissolved in ethanol. The desorbed macroporous resin is rinsed with deionized water and then used for the next adsorption of seaweed polyphenols; the ethanol in the desorption pool can be used repeatedly to achieve the purpose of enriching seaweed polyphenols.

(5)上述解吸附的乙醇溶液于40℃下减压浓缩至干,然后采用真空干燥于50℃干燥2h,得到高纯度海藻多酚粉末18.4g,产品总酚含量为91.5质量%。(5) The above-mentioned desorbed ethanol solution was concentrated to dryness under reduced pressure at 40° C., and then dried in vacuum at 50° C. for 2 hours to obtain 18.4 g of high-purity seaweed polyphenol powder with a total phenol content of 91.5% by mass.

实施例2:裙带菜制备高纯度海藻多酚Embodiment 2: Preparation of high-purity seaweed polyphenols from wakame

(1)取含水量为20质量%干裙带菜1kg,用自来水浸泡、漂洗、打浆,得到海藻浆0.55L;送入搅拌器后加入2.75L去离子水,温下以120转/min转速搅拌30min;然后以1000转/min离心5min,分别收集上清液和海藻渣;重复上述步骤,上清液用于制备海藻多糖;收集得到海藻渣313g,用于提取制备海藻多酚。(1) Take 1 kg of dried wakame with a water content of 20% by mass, soak, rinse, and beat with tap water to obtain 0.55 L of seaweed pulp; add 2.75 L of deionized water after sending it into the agitator, and stir at a speed of 120 rpm under temperature 30 min; then centrifuge at 1000 rpm for 5 min, collect the supernatant and seaweed residue respectively; repeat the above steps, the supernatant is used to prepare seaweed polysaccharide; collect 313 g of seaweed residue, which is used to extract and prepare seaweed polyphenols.

(2)取上述湿裙带菜渣与1.565g复合酶混合均匀,室温下水解5h,实现海藻细胞壁破壁。(2) Mix the above-mentioned wet wakame residue with 1.565 g of compound enzyme evenly, and hydrolyze it at room temperature for 5 hours, so as to break the cell wall of seaweed.

(3)采用含0.05质量%、0.01体积%植酸及0.1体积%醋酸的80体积%乙醇水溶液为提取液。1.565L提取液加入到上述酶解破壁的海藻渣中并混匀,室温下提取1.5h;以3000转/min离心5min,分别收集上清液和海藻渣。重复前述步骤进行二次提取。海藻渣经干燥后用于饲料添加剂原料;合并两次上清液3.0L,用于海藻多酚的分离纯化。(3) 80% by volume ethanol aqueous solution containing 0.05% by mass, 0.01% by volume of phytic acid and 0.1% by volume of acetic acid is used as the extract. Add 1.565L of the extract to the above-mentioned enzymatically broken seaweed residue and mix well, extract at room temperature for 1.5h; centrifuge at 3000 rpm for 5min, and collect the supernatant and seaweed residue respectively. Repeat the previous steps for the second extraction. Seaweed dregs were dried and used as raw materials for feed additives; 3.0 L of the two supernatants were combined for separation and purification of seaweed polyphenols.

(4)将上述上清液倒入装有硅胶的吸附池脱色2h;在40℃下将上清液减压浓缩至1.5L体积后,用国产XDA-7大孔吸收树脂固相萃取2h;大孔树脂用去离子水快速漂洗后,用食品级无水乙醇解吸附,得到富含海藻多酚的乙醇溶液。(4) Pour the above supernatant into an adsorption tank equipped with silica gel for decolorization for 2 hours; after concentrating the supernatant under reduced pressure to a volume of 1.5 L at 40° C., use domestic XDA-7 macroporous absorption resin for solid-phase extraction for 2 hours; After the macroporous resin is quickly rinsed with deionized water, it is desorbed with food-grade absolute ethanol to obtain an ethanol solution rich in seaweed polyphenols.

(5)上述解吸附的乙醇溶液于40℃下减压浓缩至干,然后采用真空干燥于50℃干燥2h,得到高纯度海藻多酚粉末27.6g,产品总酚含量为93.2质量%。(5) The above-mentioned desorbed ethanol solution was concentrated to dryness under reduced pressure at 40° C., and then dried in vacuum at 50° C. for 2 hours to obtain 27.6 g of high-purity seaweed polyphenol powder with a total phenol content of 93.2% by mass.

实施例3:海黍子制备高纯度海藻多酚Embodiment 3: Sea millet prepares high-purity seaweed polyphenols

(1)取含水量为20质量%干海黍子1kg,用自来水浸泡、漂洗、打浆,得到海藻浆0.5L;送入搅拌器后加入2.5L去离子水,温下以120转/min转速搅拌30min;然后以1000转/min离心5min,分别收集上清液和海藻渣;重复上述步骤,上清液用于制备海藻多糖;收集得到海藻渣410g,用于提取制备海藻多酚。(1) Take 1 kg of dry sea millet with a water content of 20% by mass, soak, rinse, and beat with tap water to obtain 0.5 L of seaweed slurry; add 2.5 L of deionized water after sending it into the agitator, and use 120 rpm under temperature. Stir for 30 minutes; then centrifuge at 1000 rpm for 5 minutes to collect the supernatant and seaweed residue; repeat the above steps, the supernatant is used to prepare seaweed polysaccharides; collect 410 g of seaweed residue, which is used to extract and prepare seaweed polyphenols.

(2)取上述湿裙带菜渣与2.05g复合酶混合均匀,室温下水解5h,实现海藻细胞壁破壁。(2) Mix the above-mentioned wet wakame residue with 2.05 g of compound enzyme evenly, and hydrolyze it at room temperature for 5 hours, so as to break the cell wall of seaweed.

(3)采用含0.05质量%、0.01体积%植酸及0.1体积%醋酸的80体积%乙醇水溶液为提取液。2.05L提取液加入到上述酶解破壁的海藻渣中并混匀,室温下提取1.5h;以3000转/min离心5min,分别收集上清液和海藻渣。重复前述步骤进行二次提取。海藻渣经干燥后用于饲料添加剂原料;合并两次上清液3.8L,用于海藻多酚的分离纯化。(3) 80% by volume ethanol aqueous solution containing 0.05% by mass, 0.01% by volume of phytic acid and 0.1% by volume of acetic acid is used as the extract. Add 2.05L of the extract to the enzymatically broken seaweed residue and mix well, extract at room temperature for 1.5h; centrifuge at 3000rpm for 5min, and collect the supernatant and seaweed residue respectively. Repeat the previous steps for the second extraction. Seaweed dregs were dried and used as raw materials for feed additives; 3.8 L of the two supernatants were combined for separation and purification of seaweed polyphenols.

(4)将上述上清液倒入装有硅胶的吸附池脱色2h;在40℃下将上清液减压浓缩至1.9L体积后,用国产XDA-7大孔吸收树脂固相萃取2h;大孔树脂用去离子水快速漂洗后,用食品级无水乙醇解吸附,得到富含海藻多酚的乙醇溶液。(4) Pour the above supernatant into an adsorption tank equipped with silica gel for decolorization for 2 hours; after concentrating the supernatant under reduced pressure to a volume of 1.9L at 40°C, use domestic XDA-7 macroporous absorption resin for solid-phase extraction for 2 hours; After the macroporous resin is quickly rinsed with deionized water, it is desorbed with food-grade absolute ethanol to obtain an ethanol solution rich in seaweed polyphenols.

(5)上述解吸附的乙醇溶液于40℃下减压浓缩至干,然后采用真空干燥于50℃干燥2h,得到高纯度海藻多酚粉末38.5g,产品总酚含量为90质量%。(5) The above-mentioned desorbed ethanol solution was concentrated to dryness under reduced pressure at 40° C., and then dried in vacuum at 50° C. for 2 hours to obtain 38.5 g of high-purity seaweed polyphenol powder with a total phenol content of 90% by mass.

实施例4:羊栖菜制备高纯度海藻多酚Example 4: Preparation of high-purity seaweed polyphenols from Hijiki

(1)取含水量为20质量%干羊栖菜1kg,用自来水浸泡、漂洗、打浆,得到海藻浆0.65L;送入搅拌器后加入3.25L去离子水,温下以120转/min转速搅拌30min;然后以1000转/min离心5min,分别收集上清液和海藻渣;重复上述步骤,上清液用于制备海藻多糖;收集得到海藻渣350g,用于提取制备海藻多酚。(1) Take 1 kg of dry hijiki with a water content of 20% by mass, soak, rinse, and beat with tap water to obtain 0.65 L of seaweed slurry; add 3.25 L of deionized water after sending it into the mixer, and use 120 rpm under temperature. Stir for 30 minutes; then centrifuge at 1000 rpm for 5 minutes to collect the supernatant and seaweed residue; repeat the above steps, the supernatant is used to prepare seaweed polysaccharide; collect 350 g of seaweed residue, which is used to extract and prepare seaweed polyphenols.

(2)取上述湿裙带菜渣与1.75g复合酶混合均匀,室温下水解5h,实现海藻细胞壁破壁。(2) Mix the above-mentioned wet wakame residue with 1.75 g of compound enzyme, and hydrolyze it at room temperature for 5 hours to break the cell wall of seaweed.

(3)采用含0.05质量%、0.01体积%植酸及0.1体积%醋酸的80体积%乙醇水溶液为提取液。1.75L提取液加入到上述酶解破壁的海藻渣中并混匀,室温下提取1.5h;以3000转/min离心5min,分别收集上清液和海藻渣。重复前述步骤进行二次提取。海藻渣经干燥后用于饲料添加剂原料;合并两次上清液3.4L,用于海藻多酚的分离纯化。(3) 80% by volume ethanol aqueous solution containing 0.05% by mass, 0.01% by volume of phytic acid and 0.1% by volume of acetic acid is used as the extract. Add 1.75L of the extract to the enzymatically broken seaweed residue and mix well, extract at room temperature for 1.5h; centrifuge at 3000 rpm for 5min, and collect the supernatant and seaweed residue respectively. Repeat the previous steps for the second extraction. Seaweed slag was dried and used as raw material for feed additives; 3.4 L of supernatants from two times were combined for separation and purification of seaweed polyphenols.

(4)将上述上清液倒入装有硅胶的吸附池脱色2h;在40℃下将上清液减压浓缩至1.7L体积后,用国产XDA-7大孔吸收树脂固相萃取2h;大孔树脂用去离子水快速漂洗后,用食品级无水乙醇解吸附,得到富含海藻多酚的乙醇溶液。(4) Pour the above supernatant into an adsorption tank equipped with silica gel for decolorization for 2 hours; after concentrating the supernatant under reduced pressure to a volume of 1.7L at 40°C, use domestic XDA-7 macroporous absorption resin for solid-phase extraction for 2 hours; After the macroporous resin is quickly rinsed with deionized water, it is desorbed with food-grade absolute ethanol to obtain an ethanol solution rich in seaweed polyphenols.

(5)上述解吸附的乙醇溶液于40℃下减压浓缩至干,然后采用真空干燥于50℃干燥2h,得到高纯度海藻多酚粉末15.3g,产品总酚含量为94.1质量%。(5) The above-mentioned desorbed ethanol solution was concentrated to dryness under reduced pressure at 40° C., and then dried in vacuum at 50° C. for 2 hours to obtain 15.3 g of high-purity seaweed polyphenol powder with a total phenol content of 94.1% by mass.

实施例5:甘苔制备高纯度海藻多酚Example 5: Preparation of high-purity seaweed polyphenols from Radix Glycyrrhizae

(1)取含水量为20质量%干甘苔1kg,用自来水浸泡、漂洗、打浆,得到海藻浆0.8L;送入搅拌器后加入4.0L去离子水,温下以120转/min转速搅拌30min;然后以1000转/min离心5min,分别收集上清液和海藻渣;重复上述步骤,上清液用于制备海藻多糖;收集得到海藻渣280g,用于提取制备海藻多酚。(1) Take 1 kg of dry licorice with a water content of 20% by mass, soak, rinse, and beat with tap water to obtain 0.8 L of seaweed slurry; add 4.0 L of deionized water after sending it into the mixer, and stir at 120 rpm under temperature 30 min; then centrifuge at 1000 rpm for 5 min, collect the supernatant and seaweed residue respectively; repeat the above steps, the supernatant is used to prepare seaweed polysaccharide; collect 280 g of seaweed residue, which is used to extract and prepare seaweed polyphenols.

(2)取上述湿裙带菜渣与1.4g复合酶混合均匀,室温下水解5h,实现海藻细胞壁破壁。(2) Mix the above-mentioned wet wakame residue with 1.4 g of compound enzyme, and hydrolyze it at room temperature for 5 hours to break the cell wall of seaweed.

(3)采用含0.05质量%、0.01体积%植酸及0.1体积%醋酸的80体积%乙醇水溶液为提取液。1.4L提取液加入到上述酶解破壁的海藻渣中并混匀,室温下提取1.5h;以3000转/min离心5min,分别收集上清液和海藻渣。重复前述步骤进行二次提取。海藻渣经干燥后用于饲料添加剂原料;合并两次上清液2.5L,用于海藻多酚的分离纯化。(3) 80% by volume ethanol aqueous solution containing 0.05% by mass, 0.01% by volume of phytic acid and 0.1% by volume of acetic acid is used as the extract. Add 1.4L of the extract to the above-mentioned enzymatically broken seaweed residue and mix well, extract at room temperature for 1.5h; centrifuge at 3000 rpm for 5min, and collect the supernatant and seaweed residue respectively. Repeat the previous steps for the second extraction. Seaweed dregs were dried and used as raw materials for feed additives; 2.5 L of supernatants from two times were combined for separation and purification of seaweed polyphenols.

(4)将上述上清液倒入装有硅胶的吸附池脱色2h;在40℃下将上清液减压浓缩至1.25L体积后,用国产XDA-7大孔吸收树脂固相萃取2h;大孔树脂用去离子水快速漂洗后,用食品级无水乙醇解吸附,得到富含海藻多酚的乙醇溶液。(4) Pour the above supernatant into an adsorption tank equipped with silica gel for decolorization for 2 hours; after concentrating the supernatant under reduced pressure to a volume of 1.25L at 40°C, use domestic XDA-7 macroporous absorption resin for solid-phase extraction for 2 hours; After the macroporous resin is quickly rinsed with deionized water, it is desorbed with food-grade absolute ethanol to obtain an ethanol solution rich in seaweed polyphenols.

(5)上述解吸附的乙醇溶液于40℃下减压浓缩至干,然后采用真空干燥于50℃干燥2h,得到高纯度海藻多酚粉末65.2g,产品总酚含量为95质量%。(5) The above-mentioned desorbed ethanol solution was concentrated to dryness under reduced pressure at 40° C., and then dried in vacuum at 50° C. for 2 hours to obtain 65.2 g of high-purity seaweed polyphenol powder with a total phenol content of 95% by mass.

本发明针对海藻多酚易氧化降解的特点,在提取过程中通过添加保护剂提高了海藻多酚的稳定性,从而提高了提取效率。实验以酶解破壁后的海带渣为原料,对维生素C、植酸及其组成的复合制剂的保护效果进行了对比研究。海带渣与提取液(含0.1%醋酸的80%乙醇水溶液)的固定比为1:5(w:v),室温下提取1.5h,提取两次,以海藻多酚提取率判断保护剂的效果,结果如表1所示。实验结果发现,在保护剂的作用下,海藻多酚的提取率显著提高。其中,植酸的保护效果要优于维生素C,由二者组成的复合剂效果最佳。通过比较维生素C与植酸的不同浓度组合对海藻多酚的保护作用,发现0.05质量%与0.01体积%植酸的保护效果与其他组合没有显著差异。The invention aims at the characteristic that seaweed polyphenols are easy to be oxidized and degraded, and improves the stability of seaweed polyphenols by adding a protective agent during the extraction process, thereby improving the extraction efficiency. In the experiment, the protective effects of vitamin C, phytic acid and their compound preparations were comparatively studied by using the kelp slag after enzymatic hydrolysis and breaking the wall as raw materials. The fixed ratio of kelp slag and extract (80% ethanol aqueous solution containing 0.1% acetic acid) is 1:5 (w:v), extract at room temperature for 1.5h, extract twice, and judge the effect of protective agent by the extraction rate of seaweed polyphenols , and the results are shown in Table 1. The experimental results found that under the action of the protective agent, the extraction rate of seaweed polyphenols was significantly improved. Among them, the protective effect of phytic acid is better than that of vitamin C, and the compound agent composed of the two has the best effect. By comparing the protective effect of different concentration combinations of vitamin C and phytic acid on seaweed polyphenols, it was found that the protective effect of 0.05% by mass and 0.01% by volume of phytic acid was not significantly different from other combinations.

表1保护剂对海藻多酚提取率的影响Table 1 The influence of protective agent on the extraction rate of seaweed polyphenols

总之,本发明基于对海藻的全藻资源利用,通过添加保护剂减少生产过程对海藻多酚的破坏,采用生物酶破壁-固相萃取联用技术实现制备海藻多酚的高效率、高纯度目标,减少传统工艺中的柱层析等单元操作,具有绿色环保、低能高效等技术优势。In a word, the present invention is based on the utilization of the whole algae resources of seaweed, reduces the damage to seaweed polyphenols in the production process by adding protective agents, and adopts the combination technology of biological enzyme wall breaking and solid phase extraction to achieve high efficiency and high purity of seaweed polyphenols The goal is to reduce unit operations such as column chromatography in traditional processes, and has technical advantages such as green environmental protection, low energy and high efficiency.

尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在不脱离本发明的原理和宗旨的情况下在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。Although the embodiments of the present invention have been shown and described above, it can be understood that the above embodiments are exemplary and cannot be construed as limitations to the present invention. Variations, modifications, substitutions, and modifications to the above-described embodiments are possible within the scope of the present invention.

Claims (7)

1.一种高纯度海藻多酚的制备方法,其特征在于:包括以下步骤:1. A preparation method for high-purity seaweed polyphenols, characterized in that: comprises the following steps: 步骤一、海藻多糖与海藻渣的分离:首先将含水量为20%的干海藻用自来水浸泡,漂洗除去泥沙杂质后用打浆机打浆;海藻浆送入搅拌机中,并按海藻浆:去离子水体积比为1:5加入去离子水,室温下以120转/min转速搅拌30分钟;海藻浆用低速离心机以1000转/min的转速离心5min,分别收集上清液和海藻渣;海藻渣按上述步骤及条件经搅拌机搅拌、离心机离心处理后,再次分别收集上清液和海藻渣;合并两次上清液,经喷雾干燥后得到海藻多糖;收集海藻渣,用于提取制备海藻多酚;Step 1. Separation of seaweed polysaccharides and seaweed residue: first soak the dried seaweed with a water content of 20% in tap water, rinse to remove sediment impurities, and beat with a beater; send the seaweed pulp into the mixer, and press the seaweed pulp: deionized The water volume ratio is 1:5, add deionized water, stir at room temperature at 120 rpm for 30 minutes; use a low-speed centrifuge to centrifuge the seaweed slurry at 1000 rpm for 5 minutes, and collect the supernatant and seaweed residue; After the slag is stirred by a mixer and centrifuged in a centrifuge according to the above steps and conditions, the supernatant and seaweed residue are collected separately again; the two supernatants are combined and spray-dried to obtain seaweed polysaccharide; the seaweed residue is collected for extraction and preparation of seaweed polyphenols; 步骤二、海藻渣的酶解破壁:将由纤维素酶与果胶酶按重量比1:1组成的复合酶按重量比为1:1000加入到所述海藻渣中,室温下水解5h,实现海藻细胞壁破壁;Step 2. Enzymatic hydrolysis of seaweed dregs: add a compound enzyme composed of cellulase and pectinase in a weight ratio of 1:1000 to the seaweed dregs, and hydrolyze for 5 hours at room temperature to achieve Algae cell wall breakdown; 步骤三、海藻多酚的高效提取:将海藻多酚保护剂溶解于去离子水中,然后与食品级无水乙醇按体积比为1:4混合,并按体积比加入醋酸,使醋酸终体积浓度为0.1%,混匀后为海藻多酚的提取液;所述提取液与海藻渣按体积/重量比为5:1进行混匀,室温下提取1.5h,以3000转/min的转速离心5min,分别收集上清液和海藻渣;海藻渣继续用所述提取液重复前述步骤进行二次提取,分别收集上清液和海藻渣;海藻渣经干燥后用于饲料添加剂原料;合并两次上清液,用于海藻多酚的分离纯化;Step 3. High-efficiency extraction of seaweed polyphenols: dissolve the seaweed polyphenol protective agent in deionized water, then mix it with food-grade absolute ethanol at a volume ratio of 1:4, and add acetic acid according to the volume ratio to make the final volume concentration of acetic acid 0.1%, after mixing, it is the extract of seaweed polyphenols; the extract and seaweed residue are mixed at a volume/weight ratio of 5:1, extracted at room temperature for 1.5h, and centrifuged at 3000 rpm for 5min , collect supernatant and seaweed residue respectively; seaweed residue continues to use the extract to repeat the above steps for secondary extraction, collect supernatant and seaweed residue respectively; seaweed residue is used as feed additive raw material after being dried; Serum, used for the separation and purification of seaweed polyphenols; 步骤四、海藻多酚的分离纯化:将步骤三制得的上清液倒入含有硅胶的吸附池进行静态吸附脱色2h,硅胶吸附的色素进一步用于制备岩藻黄质活性物质;然后采用减压浓缩法在40℃下将海藻多酚提取液浓缩至50%体积后,采用国产XDA-7大孔吸收树脂对海藻多酚进行固相萃取2h;将XDA-7大孔树脂用去离子水快速漂洗,除去糖、小肽杂质;然后将XDA-7大孔树脂用食品级无水乙醇浸泡0.5h,将吸附于大孔树脂上的海藻多酚洗脱并溶解于乙醇中,得到乙醇浸泡液;Step 4. Separation and purification of seaweed polyphenols: pour the supernatant obtained in step 3 into an adsorption pool containing silica gel for static adsorption and decolorization for 2 hours, and the pigment adsorbed by silica gel is further used to prepare fucoxanthin active substances; After the seaweed polyphenol extract was concentrated to 50% volume at 40°C by the pressure concentration method, the seaweed polyphenol was subjected to solid-phase extraction with domestic XDA-7 macroporous absorption resin for 2 hours; the XDA-7 macroporous resin was deionized water Rinse quickly to remove sugar and small peptide impurities; then soak the XDA-7 macroporous resin in food-grade anhydrous ethanol for 0.5h, elute the seaweed polyphenols adsorbed on the macroporous resin and dissolve them in ethanol to obtain ethanol-soaked liquid; 步骤五、海藻多酚的制备:将所述乙醇浸泡液在40℃下减压浓缩至干,在50℃下真空干燥2h,得到海藻多酚产品。Step 5, preparation of seaweed polyphenols: the ethanol soaking solution was concentrated to dryness under reduced pressure at 40° C., and vacuum-dried at 50° C. for 2 hours to obtain seaweed polyphenol products. 2.如权利要求1所述的一种高纯度海藻多酚的制备方法,其特征在于:所述海藻为海带、裙带菜、羊牺菜、海黍子、鼠尾藻和甘苔中的至少一种。2. the preparation method of a kind of high-purity seaweed polyphenol as claimed in claim 1, is characterized in that: described seaweed is at least one in kelp, wakame, hibiscus, sea millet, sargassum and licorice . 3.如权利要求1所述的一种高纯度海藻多酚的制备方法,其特征在于:所述步骤三的海藻多酚保护剂为维生素C或植酸或由维生素C与植酸组成的复合物。3. The preparation method of a kind of high-purity seaweed polyphenols as claimed in claim 1, characterized in that: the seaweed polyphenol protective agent in the step 3 is vitamin C or phytic acid or a compound composed of vitamin C and phytic acid thing. 4.如权利要求1所述的一种高纯度海藻多酚的制备方法,其特征在于:所述步骤三的提取液中含有质量体积比为0.05-0.5%的维生素C。4. A method for preparing high-purity seaweed polyphenols as claimed in claim 1, characterized in that: the extract in step 3 contains vitamin C with a mass-volume ratio of 0.05-0.5%. 5.如权利要求1所述的一种高纯度海藻多酚的制备方法,其特征在于:所述步骤三的提取液中含有体积比为0.01-0.1%的植酸。5 . The method for preparing high-purity seaweed polyphenols according to claim 1 , wherein the extract in step 3 contains 0.01-0.1% phytic acid by volume. 6.如权利要求1所述的一种高纯度海藻多酚的制备方法,其特征在于:所述步骤三的提取液中含有质量体积比为0.05-0.1%的维生素C及体积比为0.01-0.05%的植酸。6. A method for preparing high-purity seaweed polyphenols as claimed in claim 1, characterized in that: the extract in the step 3 contains vitamin C with a mass-volume ratio of 0.05-0.1% and a volume ratio of 0.01- 0.05% Phytic Acid. 7.如权利要求1所述的一种高纯度海藻多酚的制备方法,其特征在于:所述海藻多酚产品为白色粉末;所述海藻多酚的提取率为1.5-6.5%;纯度为90-95%。7. a kind of preparation method of high-purity seaweed polyphenol as claimed in claim 1 is characterized in that: described seaweed polyphenol product is white powder; The extraction rate of described seaweed polyphenol is 1.5-6.5%; Purity is 90-95%.
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