WO2020073975A1 - 一种工业化提取万寿菊黄酮的方法及其万寿菊黄酮 - Google Patents

一种工业化提取万寿菊黄酮的方法及其万寿菊黄酮 Download PDF

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WO2020073975A1
WO2020073975A1 PCT/CN2019/110502 CN2019110502W WO2020073975A1 WO 2020073975 A1 WO2020073975 A1 WO 2020073975A1 CN 2019110502 W CN2019110502 W CN 2019110502W WO 2020073975 A1 WO2020073975 A1 WO 2020073975A1
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marigold
flavonoids
extract
extracting
concentration
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French (fr)
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高伟
连运河
吴迪
王欢欢
冀云武
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晨光生物科技集团股份有限公司
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00—Antineoplastic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P37/00—Drugs for immunological or allergic disorders
    • A61P37/08—Antiallergic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00—General protective or antinoxious agents
    • A61P39/06—Free radical scavengers or antioxidants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00—Drugs for disorders of the cardiovascular system
    • A61P9/06—Antiarrhythmics
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00—Drugs for disorders of the cardiovascular system
    • A61P9/12—Antihypertensives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/55—Liquid-liquid separation; Phase separation

Definitions

  • the invention relates to the technical field of plant functional component extraction, in particular to a method for extracting flavonoids from marigold.
  • Marigold is one of the main cultivated potted plants in China, and it is widely used in indoor and outdoor environment layout. With the development of nutrition and health industry, the international demand for marigold is increasing. Marigold not only has ornamental value, but also has very good medicinal value. Its main pharmacological components are flavonoids, carotenoids, terpenes, glycosides, essential oils and other components.
  • Marigold flower is the main source of lutein. After extracting lutein, a large amount of marigold residue is discarded as industrial waste or used as feed. This has a certain impact on the environment and also causes a lot of waste of resources.
  • there are some other active ingredients in marigold flowers such as oligosaccharides, glycosides and other compounds to be developed.
  • there is a scheme for utilizing marigold flavonoids in marigold flower meal but there are problems of complicated process flow and high cost in the process of industrial production.
  • the object of the present invention is to provide an industrial method for extracting flavonoids from marigold, including the following steps:
  • the degree of concentration of the extract is to control the content of solids in the supernatant to be 5-30%.
  • the extract is mainly ethanol, and in order to improve the purity of marigold flavonoids, ultrasound and repeated extraction operations are usually required, but this is used in industrial applications. Will greatly increase costs.
  • the present invention found that the extraction of marigold flower meal with methanol solution can fully extract the flavonoids of marigold, and the flavones of marigold can be precipitated by concentration, and the degree of concentration can be strictly controlled during the precipitation process, which can fully Extraction and better purification, the resulting extract has better biological efficacy.
  • the marigold flower meal in the present invention is the residue remaining after extracting lutein from marigold flower or marigold flower particles.
  • the marigold flower granules are prepared by fermenting marigold flowers, pressing, drying, crushing and granulating.
  • the degree of concentration of the extract is controlled by controlling the content of solids in the supernatant to be 10-30%.
  • the method for determining the end point of concentration is to centrifuge the concentrated extract, and the solid content of the supernatant obtained after centrifugation is equal to the solid content in the supernatant after filtration.
  • the solid content of the supernatant obtained after centrifugation is measured to determine the solid content of the supernatant after filtration.
  • the volume fraction of the methanol solution is 80-90%.
  • the extracted flavonoids have higher purity and higher biological activity.
  • the mass-volume ratio of the marigold flower meal to the methanol solution is 1: 7-20, more preferably 1: 7-10.
  • the flavonoids of marigold can be fully extracted with a high extraction rate.
  • the extraction is performed under conditions of a temperature of 50-70 ° C.
  • a temperature of 50-70 ° C At the above temperature, marigold flavonoids can be fully and completely extracted. If the temperature is too low, the extraction of marigold flavonoids is insufficient, and if the temperature is too high, the extraction yield of marigold flavonoids will not increase.
  • the specific conditions for the concentration are: a temperature of 60 to 90 ° C.
  • the pore size of the filter cloth is 300-500 mesh.
  • the filtering pressure is 0.1 to 0.6 MPa.
  • a methanol solution with a volume fraction of 80 to 90% is used, and the extraction solution is obtained under the condition of a temperature of 50 to 70 ° C according to the mass volume ratio of marigold flower meal to the methanol solution of 1: 7 to 10;
  • the degree of concentration is to control the content of solids in the supernatant to be 10-30%.
  • the present invention further includes the operation of extracting the water-soluble polyphenols in the supernatant, including the steps of: adsorbing the supernatant through a polar macroporous adsorption resin, and absorbing the polar macroporous resin Perform analysis, collect the analysis solution and concentrate and dry it to obtain water-soluble polyphenols.
  • the macroporous resin is any one of D101, DM130, LX-5, LX-312, and LX-158.
  • the above macroporous resin was purchased from Xi'an Lanxiao Technology Co., Ltd.
  • the analysis liquid used in the analysis is one or a mixture of n-hexane, methanol, acetonitrile, ethanol, and water.
  • the polar macroporous adsorption resin is LX-158 or LX-5, and the analysis solution is ethanol with a concentration of 70-75%.
  • Another object of the present invention is to protect the marigold flavonoids prepared by the method of the present invention.
  • the total content of flavonoids is greater than 80%.
  • the invention also protects the water-soluble polyphenols prepared by the method of the invention.
  • the total content of polyphenols is greater than 50%.
  • the present invention proposes a method for simply extracting marigold flavonoids, which only includes the operations of extraction, concentration and filtration. Compared with other solutions in the prior art, the extraction method of the present invention has short steps, low cost and is applicable For industrial mass production.
  • the present invention selects methanol as the extractant to extract the flavonoids of marigold. Compared with other alcohol extractants, the methanol extraction efficiency is high, and the longevity can be achieved after less repetition The full extraction of chrysanthemum flavone can effectively reduce the cost in industrial production.
  • the active ingredients in marigold flavonoids can be fully extracted.
  • the purity of the obtained marigold flavonoids is more than 80%, and the maximum yield of the extract is more than 8%.
  • the present invention further proposes a method for extracting marigold polyphenols.
  • This method has simple steps, low cost, and a purity of about 50%.
  • the extracted water-soluble polyphenols have good antioxidant activity and DPPH antioxidant activity
  • the IC50 value can be as low as 12.5 ⁇ g / ml, and the IC50 value for ABTS scavenging activity can be as low as 15.5 ⁇ g / ml.
  • the marigold flower meal used in the examples is the residue obtained after extracting the lutein in the marigold particles with n-hexane and drying.
  • the marigold flower particles are prepared after fermentation of marigold flowers, followed by pressing, drying, crushing and granulation.
  • This embodiment relates to a method for extracting flavonoids from marigold, which includes the following steps:
  • the extract is concentrated under pressure at a vacuum of 0.07 ⁇ 0.002Mpa and a temperature of 70 ° C.
  • the concentrated extract is centrifuged and the supernatant is taken. After testing, the solid content in the supernatant is 10 %, At this time, the volume of the concentrated solution is 35L;
  • This embodiment relates to a method for extracting flavonoids from marigold, which includes the following steps:
  • the extract is concentrated under pressure at a vacuum of 0.07 ⁇ 0.002Mpa and a temperature of 90 ° C, and concentrated until the concentrated extract is centrifuged and the supernatant is taken. After detection, the solid content in the supernatant is detected 30%, at this time, the volume of the concentrated solution is 40L;
  • the concentrated liquid is subjected to plate and frame filtration, the concentrated liquid is passed through a filter cloth with a pore size of 500 mesh, the pressure in the filtering process is 0.3 Mpa, and the filter cake is dried to obtain marigold flavonoids.
  • This embodiment relates to the method for extracting water-soluble polyphenols according to the present invention, which includes the following steps:
  • Example 1 Take the clear solution obtained in step 3) of Example 1, load the clear solution onto the macroporous resin LX-158, control the flow rate 1BV / h, analyze the resin with 75% ethanol solution, and concentrate and dry the analysis solution to obtain water-soluble longevity Chrysanthemum polyphenols.
  • This embodiment relates to the method for extracting water-soluble polyphenols according to the present invention, which includes the following steps:
  • step 1) 60% ethanol is used to extract marigold flower meal, and other operations are the same as in Example 1.
  • step 1) 90% ethanol is used to extract marigold flower meal, and other operations are the same as in Example 1.
  • step 1) 60% methanol is used to extract marigold flower meal, and other operations are the same as those in Example 1.
  • step 1) the concentration is 20L, the concentrated extract is centrifuged, and the supernatant is taken. After detection, the solid content in the supernatant is 40%, other The operation is the same as in Example 1.
  • Example 1 Compared with Example 1, the difference is that the extraction condition in step 1) is a material-liquid ratio of 1: 5, and other operations are the same as those in Example 1.
  • This comparative example uses the following steps to extract:
  • the yield and purity of the extracted marigold flavonoids are high, and its performance in antioxidant activity is very outstanding.
  • the extracted water-soluble polyphenols also have good antioxidant activity. If the method of this application is not used.
  • ethanol with a concentration of 60% is used as the extraction solution, the yield, purity, and content of the extract are significantly reduced, and the decrease in its antioxidant activity is very obvious.
  • the concentration of 90% is used. The same is true for ethanol, and it is not ideal to use methanol with a concentration of 60% in Comparative Example 3.
  • the determination of the end point of concentration in this application is also very important.
  • Comparative Example 4 the solid content in the clear solution is concentrated to 40%. Although the yield of flavonoids has increased, its purity and biological activity have decreased significantly. .
  • the comparative example 5 does not use the material-liquid ratio described in this application, and its extraction rate is significantly reduced. The effect of adjusting the extraction method in Comparative Example 6 will be much worse. In summary, under the conditions provided in this application, the yield and purity of the extracted flavonoids are high, and its antioxidant activity is very outstanding.
  • the invention provides an industrial method for extracting flavonoids from marigold.
  • the present invention uses methanol solution to extract marigold flower meal, concentrate the extract to extract all marigold flavonoids, filter to obtain clear liquid and filter cake, and dry the filter cake to obtain marigold flavonoids; concentrate to all marigold flavonoids
  • the judging criterion for precipitation is that the solid content in the clear solution is 5-30%.
  • the method of the invention has simple steps and low cost, and is suitable for industrial large-scale production.
  • the extracted marigold flavonoids have high purity, multiple biological activities, high industrial application value, and good economic value and application prospects. .

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Abstract

一种万寿菊黄酮的提取方法，其主要步骤为，利用甲醇溶液对万寿菊花粕进行提取，将提取液浓缩至固形物含量为5～30％，进行过滤，得清液和滤饼，将滤饼烘干，即得万寿菊黄酮。

Description

一种工业化提取万寿菊黄酮的方法及其万寿菊黄酮
交叉引用
本申请要求2018年10月12日提交的专利名称为“一种工业化提取万寿菊黄酮的方法及其万寿菊黄酮”的第201811188765.7号中国专利申请的优先权，其全部公开内容通过引用整体并入本文。
技术领域
本发明涉及植物功能性成分提取的技术领域，具体涉及一种万寿菊中黄酮的提取方法。
背景技术
万寿菊是我国主要栽培的草本盆花之一，且广泛用于室内外环境布置。随着营养健康产业发展，国际上对万寿菊的需求量越来越多。万寿菊不但具有观赏价值外，而且还有很好的药用价值，其起药理作用的主要成分是黄酮类物质、类胡萝卜素类、萜类、糖苷类、精油等成分。
万寿菊花是叶黄素主要来源，提取叶黄素后，大量的万寿菊渣当成工业下脚料丢弃，或作为饲料使用。这对环境造成一定的影响，而且还造成很大的资源浪费。研究报道，万寿菊花中含有丰富的黄酮类物质，如槲皮万寿菊素等，约占万寿菊花的2％～11％左右。研究表明，这些黄酮类物质具有很好的生物活性，如具有抗氧化、抗炎、抗过敏、降血压、抗心律失常、抗肿瘤等功效。同时，万寿菊花中还有一些其它有效成分，如寡糖、糖苷类等化合物有待开发。现有技术中有对万寿菊花粕中的万寿菊黄酮进行利用的方案，但是在工业化生产的过程中存在工艺流程复杂，成本高的问题。
发明内容
本发明的目的是提供一种工业化提取万寿菊黄酮的方法，包括如下步骤：
利用体积分数为70～90％的甲醇溶液对万寿菊花粕进行提取，得提取 液；
将所述提取液浓缩后进行过滤(优选为板框过滤)，得清液和滤饼，将所述滤饼烘干即得万寿菊黄酮；
所述提取液浓缩的程度为控制所述清液中固形物的含量为5～30％。
现有技术中有多种对万寿菊黄酮进行提取的方法，其提取液主要以乙醇为主，且为提高万寿菊黄酮的纯度，通常需要进行超声和反复萃取的操作，但这在工业应用中会大大提高成本。本发明发现，采用甲醇溶液对万寿菊花粕进行提取，可对万寿菊黄酮进行充分地提取，并通过浓缩使万寿菊黄酮析出，析出过程中严格控制浓缩的程度，可对万寿菊黄酮进行充分的提取以及较好的精制，所得提取物有较好的生物功效。
本发明所述万寿菊花粕为对万寿菊花或万寿菊花颗粒提取叶黄素后剩余的残渣。
所述万寿菊花颗粒由万寿菊花发酵后，进行压榨、烘干、粉碎和造粒后制得。
优选的，所述提取液的浓缩的程度以控制所述清液中固形物的含量为10～30％为准。
作为优选的操作方式，判断浓缩终点的方法为将浓缩后的提取液进行离心，离心后得到的上清液的固形物含量即等同于过滤后清液中的固形物含量，浓缩的过程中通过测定离心后所得上清液的固形物含量来判断过滤后清液中固形物的含量。
优选的，所述甲醇溶液的体积分数为80～90％。采用上述浓度的甲醇溶液，提取得到的黄酮类物质的纯度更高、生物活性更高。
优选的，所述万寿菊花粕与所述甲醇溶液的质量体积比为1:7～20，更优选1:7～10。在上述范围内，可对万寿菊黄酮进行充分地提取，提取率较高。
优选的，所述提取在温度50～70℃的条件下进行。在上述温度下，万寿菊黄酮能够得到充分完全的提取，温度过低，万寿菊黄酮提取不充分， 温度过高万寿菊黄酮的提取得率也不会增加。
优选的，所述浓缩的具体条件为：温度60～90℃。
优选的，在过滤的过程中，滤布的孔径为300～500目。
优选的，所述过滤的压力为0.1～0.6MPa。
作为优选的方案，包括如下步骤：
采用体积分数为80～90％的甲醇溶液，按照万寿菊花粕与所述甲醇溶液的质量体积比为1:7～10，在温度50～70℃的条件下进行提取，得提取液；
将所述提取液浓缩后进行过滤(优选为板框过滤)，得清液和滤饼，将所述滤饼烘干即得万寿菊黄酮；
所述浓缩的程度为控制所述清液中固形物的含量为10～30％。
作为优选的方案，包括如下步骤：
1)在温度55～65℃的条件下，用浓度为80～90％的甲醇溶液对万寿菊花粕逆流提取2～6h；控制甲醇溶液与万寿菊花粕的体积质量比为7～10:1，得提取液；
2)将提取液在温度70～90℃条件下进行加压浓缩，对浓缩后的提取液进行离心后取上清液，经检测，清液中的固形物含量为10～30％，停止浓缩，得浓缩液；
3)对所述浓缩液进行过滤，将所述浓缩液通过孔径为300～500目的滤布，过滤过程中的压力为0.1～0.6Mpa，收集清液和滤饼，将所述滤饼烘干得到万寿菊黄酮。
作为优选的方案，本发明还包括对清液中的水溶性多酚进行提取的操作，包括如下步骤：将所述清液通过极性大孔吸附树脂进行吸附，对所述极性大孔树脂进行解析，收集解析液并对其进行浓缩干燥，即得水溶性多酚。
进一步优选的，所述大孔树脂为D101、DM130、LX-5、LX-312、LX-158中的任意一种。上述大孔树脂购自西安蓝晓科技有限公司。
优选的，所述解析使用的解析液为正己烷、甲醇、乙腈、乙醇、水中的一种或几种的混合液。
优选的，所述极性大孔吸附树脂为LX-158或LX-5，所述解析液为浓度70～75％的乙醇。
本发明的另一目的是保护本发明所述方法制备得到的万寿菊黄酮。
优选的，其中黄酮类物质的总含量大于80％。
本发明还保护本发明的方法制备得到的水溶性多酚。
优选的，其中多酚类物质的总含量大于50％。
本发明的方案具有如下有益效果：
1)本发明提出了一种简单地提取万寿菊黄酮的方法，仅包括提取、浓缩和过滤的操作，与现有技术中的其他方案相比，本发明的提取方法步骤短、成本低，适用于工业化大规模生产。
2)针对于万寿菊花粕，本发明选择甲醇作为提取剂对万寿菊黄酮进行提取，与选用其他醇类的提取剂相比，甲醇的提取效率高，经过较少的重复次数即可实现对万寿菊黄酮的充分提取，可有效地降低工业生产中的成本。
3)采用本发明的方法，可对万寿菊黄酮中的有效成分进行充分提取，所得万寿菊黄酮的纯度为80％以上，提取物得率最高为8％以上，而且提取到的万寿菊黄酮具有很好的抗氧化功效、抑菌效果以及促肉鸡生长的功效。
4)本发明还进一步提出了万寿菊多酚的提取方法，这种方法步骤简单，成本低，纯度为50％左右，提取得到的水溶性多酚具有较好的抗氧化活性，DPPH抗氧化活力的IC50值可低至12.5μg/ml，对ABTS的清除活力的IC50值可低至15.5μg/ml。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例中所用的万寿菊花粕是正己烷提取万寿菊颗粒中的叶黄素后 烘干后所得残渣。所述万寿菊花颗粒为万寿菊花发酵后，进行压榨、烘干、粉碎和造粒后制得。
实施例1
本实施例涉及一种提取万寿菊黄酮的方法，包括如下步骤：
1)取万寿菊花粕50kg，加入浓度为90％的甲醇溶液350L，在60℃条件下，通过逆流萃取方式提取4h。
2)将提取液在真空度0.07±0.002Mpa，温度70℃条件下进行加压浓缩，对浓缩后的提取液进行离心后取上清液，经检测，上清液中的固形物含量为10％，此时，浓缩液的体积为35L；
3)对所述浓缩液进行板框过滤，将所述浓缩液通过孔径为300目的滤布，过滤过程中的压力为0.5Mpa，收集清液和滤饼，将所述滤饼烘干得到万寿菊黄酮。
实施例2
本实施例涉及一种提取万寿菊黄酮的方法，包括如下步骤：
1)取万寿菊花粕50kg，加入浓度为80％的甲醇溶液500L，在60℃条件下，通过逆流提取的方式提取2h。
2)将提取液在真空度0.07±0.002Mpa，温度90℃条件下进行加压浓缩，浓缩至对浓缩后的提取液进行离心后取上清液，经检测，上清液中的固形物含量为30％，此时，浓缩液的体积为40L；
3)对所述浓缩液进行板框过滤，将所述浓缩液通过孔径为500目的滤布，过滤过程中的压力为0.3Mpa，将所述滤饼烘干得到万寿菊黄酮。
实施例3
本实施例涉及本发明所述水溶性多酚的提取方法，包括如下步骤：
取实施例1步骤3)中所得清液，将所得清液上样至大孔树脂LX-158，控制流速1BV/h，利用75％乙醇溶液对树脂进行解析，解析液浓缩干燥得到水溶性万寿菊多酚。
实施例4
本实施例涉及本发明所述水溶性多酚的提取方法，包括如下步骤：
取实施例2步骤3)中所得清液，将所得清液上样至大孔树脂LX-5，控制流速0.5BV/h，利用70％的乙醇溶液对树脂进行解析，解析液浓缩干燥得到水溶性万寿菊多酚。
对比例1
与实施例1相比，其区别在于，所述步骤1)中采用浓度为60％乙醇对万寿菊花粕进行提取，其他操作与实施例1相同。
对比例2
与实施例1相比，其区别在于，所述步骤1)中采用浓度为90％乙醇对万寿菊花粕进行提取，其他操作与实施例1相同。
对比例3
与实施例1相比，其区别在于，所述步骤1)中采用浓度为60％甲醇对万寿菊花粕进行提取，其他操作与实施例1相同。
对比例4
与实施例1相比，其区别在于，所述步骤1)中浓缩至20L，对浓缩后的提取液进行离心后取清液，经检测，上清液中的固形物含量为40％，其他操作与实施例1相同。
对比例5
与实施例1相比，其区别在于，所述步骤1)中提取的条件为，料液比1：5，其他操作与实施例1相同。
对比例6
本对比例采用如下步骤进行提取：
1)取万寿菊花粕50kg，加入浓度为90％的甲醇溶液350L，在60℃条件下，通过逆流萃取方式提取4h。
2)将提取液进行板框过滤，清液在真空度0.07±0.002Mpa，温度70℃条件下进行加压浓缩，直到酒精度0，然后再进行板框过滤，取滤饼得万寿菊黄酮，其中加压浓缩和板框过滤的条件与实施例1相同。
实验例1
分别采用高效液相和紫外法对得到的万寿菊黄酮和水溶性多酚的含量分别进行检测。并对其DPPH、ABTS的清除效力进行检测，以其得率、纯度以及抗氧化活性为指标进行筛查，所得结果如表1：
表1
Figure PCTCN2019110502-appb-000001
由以上实施例和对比例可以看出，采用本发明的方法，提取得到的万寿菊黄酮的得率和纯度较高，而且其在抗氧化活性方面的性能十分突出。提取得到的水溶性多酚也具有良好的抗氧化活性。而若不采用本申请的方法。如对比例1中采用浓度为60％的乙醇作为提取液，提取物的得率、纯度以及含量收率明显下降，且其抗氧化活性的下降十分明显，对比例2中采用浓度为90％的乙醇的效果也是如此，对比例3中采用浓度为60％的甲醇也不理想。而且，本申请中对于浓缩终点的判断也十分重要，如对比例4中记载，浓缩至清液中固形物含量为40％，虽然黄酮的得率有所提高，但是其纯度生物活性却明显下降。对比例5中不采用本申请所述的料液比，其 提取率有明显的下降。对比例6中调整提取的方法，效果也会差很多。综上，在本申请所提供的条件下，提取得到的黄酮的得率和纯度高，且其抗氧化活性十分突出。
虽然，上文中已经用一般性说明、具体实施方式及试验，对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。
工业实用性
本发明提供一种工业化提取万寿菊黄酮的方法。本发明利用甲醇溶液对万寿菊花粕进行提取，将提取液浓缩至万寿菊黄酮全部析出，进行过滤，得清液和滤饼，将滤饼烘干即得万寿菊黄酮；浓缩至万寿菊黄酮全部析出的判断标准为，所述清液中的固形物含量为5～30％。本发明的方法步骤简单、成本低，适用于工业化大规模生产，提取得到的万寿菊黄酮的纯度高，具有多种生物活性，具有较高的工业应用价值，具有较好的经济价值和应用前景。

Claims (10)

  1. 一种工业化提取万寿菊黄酮的方法，其特征在于，包括如下步骤：
    利用体积分数为70～90％的甲醇溶液对万寿菊花粕进行提取，得提取液；
    将所述提取液浓缩后进行过滤，得清液和滤饼，将所述滤饼烘干即得万寿菊黄酮；
    所述提取液浓缩的程度为控制所述清液中固形物的含量为5～30％。
  2. 根据权利要求1所述的方法，其特征在于，所述万寿菊花粕为对万寿菊花或万寿菊花颗粒提取叶黄素后剩余的残渣。
  3. 根据权利要求1或2所述的方法，其特征在于，所述提取液浓缩的程度为控制所述清液中固形物的含量为10～30％。
  4. 根据权利要求1～3任一项所述的方法，其特征在于，所述甲醇溶液的体积分数为80～90％。
  5. 根据权利要求4所述的方法，其特征在于，所述万寿菊花粕与所述甲醇溶液的质量体积比为1:7～20；和/或，所述提取在温度50～70℃的条件下进行。
  6. 根据权利要求1或5所述的方法，其特征在于，所述浓缩的具体条件为温度60～90℃；和/或，所述过滤的滤布孔径为300～500目，压力为0.1～0.6MPa。
  7. 根据权利要求1～6任一项所述的方法，其特征在于，还包括：将所述清液通过极性大孔吸附树脂进行吸附，对所述极性大孔树脂进行解析，收集解析液并对其进行浓缩干燥，即得水溶性多酚。
  8. 根据权利要求7所述的方法，其特征在于，所述解析使用的解析液为正己烷、甲醇、乙腈、乙醇、水中的一种或几种的混合液。
  9. 权利要求1～8任一项方法提取得到的万寿菊黄酮；优选的，其中黄酮类物质的总含量大于80％。
  10. 权利要求7或8所述的方法提取得到的水溶性多酚；优选的，其中多酚类物质的总含量大于50％。
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