WO2022183908A1 - 一种连续提取高含量万寿菊黄酮的工业化方法 - Google Patents

一种连续提取高含量万寿菊黄酮的工业化方法 Download PDF

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WO2022183908A1
WO2022183908A1 PCT/CN2022/076401 CN2022076401W WO2022183908A1 WO 2022183908 A1 WO2022183908 A1 WO 2022183908A1 CN 2022076401 W CN2022076401 W CN 2022076401W WO 2022183908 A1 WO2022183908 A1 WO 2022183908A1
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marigold
content
extraction
continuously extracting
extracting high
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PCT/CN2022/076401
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French (fr)
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吴迪
高兰兰
连运河
崔平永
秦秀斋
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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
    • A61P7/00—Drugs for disorders of the blood or the extracellular fluid
    • A61P7/02—Antithrombotic agents; Anticoagulants; Platelet aggregation inhibitors
    • 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

Definitions

  • the invention belongs to the technical field of natural plant extraction, in particular to an industrialized method for continuously extracting high-content marigold flavonoids.
  • Marigold (Tagetes erecta L) is an annual herb of the Asteraceae family. It has the functions of clearing away heat and detoxifying, resolving phlegm and relieving cough; it has fragrance and can be used as a fragrance; it has been used as antibacterial, sedative and antispasmodic before. Marigold flowers mainly contain flavonoids, glycosides, amino acids, vitamins, pigments and other components. Marigold flavonoids are yellow-green powders extracted from marigold flowers. The main component is quercetin marigold, accounting for about 80% of marigold flavonoids. Important pharmacological effects such as platelet aggregation, anti-oxidation, and anti-tumor.
  • the main method for extracting the pharmacologically active components of marigold flowers is a step-by-step extraction method, that is, firstly use hexane solvent to extract lutein, and then use solvent to treat marigold flower residue to obtain marigold flavonoid products.
  • the patent application involved adopts mixed solvent to put out lutein and marigold flavonoids at one time, followed by separation and purification, such as: in Chinese patent application 201410104645.X, propanol-potassium hydroxide two-phase solvent is used to extract From marigold petal powder, crude products of lutein and flavonoids are obtained.
  • light-shielding reaction is required, and phase separation is required after extraction.
  • Chinese patent application 201811188771.2 uses a mixed solvent of petroleum ether and acetone to extract lutein and marigold flavonoids in marigold granules.
  • the method requires a phase separation step after extraction, and the separation method selected in this scheme is to separate after adding water, the operation is relatively complicated, and high-purity marigold flavonoids are not obtained by separation.
  • the preparation method of high-purity marigold flavonoids mainly utilizes chromatographic separation.
  • Chinese patent application CN201410708334.4 discloses that high-purity marigold flavonoids are obtained by one-dimensional liquid chromatography and two-dimensional liquid chromatography.
  • the separation volume of preparative liquid chromatography is small, the equipment is expensive, and it is not suitable for industrial production.
  • Chinese patent application 201610108596.6 describes the preparation of high content of marigold flavonoids through repeated centrifugation, filtration, washing and other steps.
  • this method involves multiple steps requiring repeated operations, which is relatively cumbersome.
  • the invention provides an industrialized method capable of simply and efficiently extracting marigold flavonoids, and the content of the marigold flavonoid extract obtained by the process can reach more than 98 percent.
  • the content of the invention of the present application is an industrialized method for continuously extracting high-content marigold flavonoids, the method comprising the following steps:
  • the raw material of the marigold flower in step 1) is fresh or dry marigold flower, or various processing forms of marigold flower available in the market, such as flower meal; the 70%-100% acetone in step 2) refers to acetone.
  • the volume fraction is 70% to 100%.
  • the particle hardness is 3 ⁇ 8kg/cm 2 ;
  • the extraction temperature is 40-60°C; preferably 45-55°C; more preferably 50-55°C;
  • the mass/volume (g/mL) ratio of the marigold flower granules and the extraction solvent is not less than 1:2; preferably 1:(2-6); more preferably 1:(3-5); further preferably 1: 4;
  • the extraction mode in step 2) is preferably countercurrent extraction
  • the number of times of extraction in step 2) is not less than 4 times; preferably 4 to 7 times.
  • each extraction time is 0.5-2.5 hours, preferably 1-2 hours; more preferably 1.5 hours.
  • the volume fraction of acetone in step 2) is preferably 70-75%; or 70-80%; or 70-85%, or 70-90%; or 70-95%; or 70-100%; or 75-80% or 75-85%; or 75-90%; or 75-95%; or 75-100%; or 80-85%; or 80-90%; or 80-95%; or 80-100%; or 85%-90%; or 85%-95%; or 85%-100%; or 90-100%; or 92-99%; or 70%-99%; or 75%-99%; or 80%- 99%; or 85% to 99%; or 90% to 99%.
  • a preferred industrialized method for continuously extracting high-content marigold flavonoids of the present invention comprises the following steps:
  • the method of reducing the volume fraction of the organic solvent in the extract described in step 3) can be concentration or addition of a strong polar solvent.
  • the present invention also provides a marigold flavonoid product prepared by the above preparation process.
  • the content of flavonoids in the product is not less than 98%.
  • the method granulates the raw materials, optimizes the compression ratio of the ring die of the granulator, and creates preconditions for the large-scale extraction of high-content marigold flavonoids.
  • the compression ratio has a good effect on the specific extraction of marigold flavonoids;
  • the method can fully extract the flavonoids in chrysanthemum by controlling the extraction solvent and the volume fraction of the organic solvent in the extraction solution, and can also achieve good separation of marigold flavonoids and impurities;
  • the flavonoid content in the marigold flavonoid product obtained by the method of the present invention is greater than or equal to 98%, and can realize continuous production, high production capacity, simple operation, meet the requirements of industrialized large-scale production, realize the industrialization of the high-content marigold flavonoid product, and improve the production efficiency. Industrial benefits.
  • the specifications of the product raw materials and reagents used in each embodiment are the same, and the used granulator, extraction equipment, filtering equipment, etc. are all the same equipment.
  • Example 2 Compared with Example 1, the difference is that the compression ratio of the ring die in the step 1) is 1:1.2, and other operations are the same as those of Example 1, and the product of Example 2 is obtained.
  • Example 3 Compared with Example 1, the difference is that in the step 1) the ring die compression ratio is 1:2.2, and other operations are the same as in Example 1 to obtain the product of Example 3.
  • Example 2 Compared with Example 1, the difference is that in the step 2), 92% acetone is used to extract the marigold granules, and other operations are the same as those in Example 1, and the product of Example 4 is obtained.
  • Example 1 Compared with Example 1, the difference is that in the step 2), 70% acetone is used to extract the marigold granules, and other operations are the same as those in Example 1, and the product of Example 5 is obtained.
  • Example 6 Compared with Example 1, the difference is that in the step 2), 100% acetone is used to extract the marigold granules, and other operations are the same as those in Example 1, and the product of Example 6 is obtained.
  • Example 7 Compared with Example 1, the difference is that the step 3) is concentrated to a volume fraction of acetone of 30%, and other operations are the same as in Example 1, and the product of Example 7 is obtained.
  • Example 8 Compared with Example 1, the difference lies in that the step 3) is concentrated to a volume fraction of acetone of 0% (that is, concentrated to no acetone in the solution), other operations are the same as those of Example 1, and the product of Example 8 is obtained.
  • Example 9 Compared with Example 1, the difference is that in the step 3), an aqueous solution is added, and the volume fraction of acetone is adjusted to 10%. Other operations are the same as those in Example 1, and the product of Example 9 is obtained.
  • Example 1 Compared with Example 1, the difference is that the compression ratio of the ring die in the step 1) is 1:3.0, and other operations are the same as those of Example 1, and the product of Comparative Example 1 is obtained.
  • Example 2 Compared with Example 1, the difference is that in the step 2), 65% acetone is used to extract the marigold granules, and other operations are the same as those in Example 1, and the product of Comparative Example 2 is obtained.
  • Example 3 Compared with Example 1, the difference is that the step 3) is concentrated to a volume fraction of acetone of 40%, and other operations are the same as in Example 1, and the product of Comparative Example 3 is obtained.
  • Example 1 Compared with Example 1, the difference is that in the step 3), the solvent is not adjusted after extraction, and it is directly concentrated and dried to obtain the product of Comparative Example 4.
  • Example 1 99.67% 98.45%
  • Example 2 98.54% 97.37%
  • Example 3 98.13% 96.12%
  • Example 4 99.17% 96.53%
  • Example 5 92.34% 96.32%
  • Example 6 99.70% 95.42%
  • Example 7 98.90% 95.60%
  • Example 8 95.34% 98.10%
  • Example 9 99.30% 98.20% Comparative Example 1 81.12% 85.10% Comparative Example 2 78.92% 81.30% Comparative Example 3 89.51% 97.70% Comparative Example 4 60.54% 98.30%
  • the above-mentioned marigold flavonoids content determination method is:
  • the marigold flavonoid samples prepared in the examples and comparative examples were dissolved in ethanol to volume, add 1 ml of 5% sodium nitrite solution, shake well, leave for 6 minutes, add 1 ml of 10% aluminum nitrate solution, shake well, leave for 6 minutes, and hydrogenate
  • Add 10ml of sodium oxide test solution add water to the scale, shake well, and leave for 15min.
  • the yield technique method is:
  • the yield of marigold flavonoids (%) (total product weight ⁇ product detection content) ⁇ 100% / (raw material total weight ⁇ raw material detection content)
  • the invention provides an industrialized method for continuously extracting high-content marigold flavonoids, which comprises the following steps: 1) granulating marigold flower raw materials, and the compression ratio of the ring die of the granulator is 1:(1.2-2.2); 2) using 70%-100% of acetone is used as an extractant to extract the above-mentioned marigold flower particles, and filter to obtain an extract; 3) reduce the volume fraction of acetone to 0-30%, filter to obtain a filter cake, and dry the filter cake to obtain marigold flavonoid products.
  • the method of the invention is simple, continuous, strong in operability, high in production capacity and low in energy consumption, suitable for industrial production, and has good economic value and application prospect.

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Abstract

一种连续提取高含量万寿菊黄酮的工业化方法及其所得万寿菊黄酮产品。所述方法包括如下步骤:1)将万寿菊花原料进行造粒，造粒机环模压缩比为1：（1.2～2.2）；2)以70％-100％的丙酮作为提取剂对上述万寿菊花颗粒进行提取，过滤，得提取液；3)下调丙酮的体积分数在0～30％，过滤，得滤饼，滤饼烘干得到万寿菊黄酮产品。本方法简单，连续性和可操作性强，产能高，能耗少，适合工业化生产。

Description

一种连续提取高含量万寿菊黄酮的工业化方法
交叉引用
本申请要求2021年3月3日提交的专利名称为“一种连续提取高含量万寿菊黄酮的工业化方法”的第202110232550.6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
本发明属于天然植物提取技术领域，具体涉及一种连续提取高含量万寿菊黄酮的工业化方法。
背景技术
万寿菊(Tagetes erecta L)为菊科万寿菊属一年生草本植物。具有清热解毒，化痰止咳；有香味，可作芳香剂；以前曾用作抑菌、镇静、解痉剂。万寿菊花主要含有黄酮类化合物、苷类、氨基酸、维生素、色素等成分。万寿菊黄酮是从万寿菊花中提取获得的黄绿色粉末，其主要的成分为槲皮万寿菊素，约占万寿菊黄酮80％左右，具有抗炎、抗过敏，降血压、抗心律失常、抗血小板凝聚，抗氧化，抗肿瘤等重要的药理作用。
目前万寿菊花中药理活性成分提取的主要方法,为分步提取法,即首先使用已烷类溶剂将叶黄素进行提取,然后利用溶剂处理万寿菊花渣得到万寿菊黄酮类产品。此外，有涉及到的专利申请采取混合溶剂一次性将叶黄素和万寿菊黄酮提出出来,后续再进行分离提纯,如:中国专利申请201410104645.X中采用丙醇-氢氧化钾双水相溶剂进行提取万寿菊花瓣粉末,获得叶黄素和黄酮粗产品。该技术方案中需要进行避光反应，并且提取后需要相的分离。又如，中国专利申请201811188771.2采用石油醚和丙酮的混合溶剂提取万寿菊颗粒中的叶黄素和万寿菊黄酮。该方法提取后需要进行相的分离步骤，且该方案中选用的分离方式为加入水后进行分离，操作较为复杂，而且未分离得到高纯度的万寿菊黄酮。
现有技术中关于高纯度万寿菊黄酮的制备方法主要利用色谱分离。如 中国专利申请CN201410708334.4公开通过一维液相色谱和二维液相色谱法提取得到高纯度的万寿菊黄酮。然而，制备液相色谱的分离量小，设备价格昂贵，不适应工业化生产。中国专利申请201610108596.6中记载通过反复离心、过滤、洗涤等步骤，制备高含量的万寿菊黄酮。但是，该方法涉及多步需要重复操作的步骤，较为繁琐。
可见为了获得高含量的万寿菊黄酮，现有技术通常需要较复杂的纯化步骤才能实现，这些复杂的工艺成本高，并不适应工业化生产的要求，目前还未见通过简单萃取、浓缩、过滤、烘干得到含量≥98％的万寿菊黄酮产品的报导。
发明内容
为克服现有万寿菊黄酮提取操作复杂，产品纯度低等缺陷。本发明提供了一种能够简单、高效提取万寿菊黄酮的工业化方法，并且通过该工艺获得的万寿菊黄酮提取物的含量可达98％以上。
本申请的发明内容为一种连续提取高含量万寿菊黄酮的工业化方法，该方法包括以下步骤：
1)使用造粒机对万寿菊花原料进行造粒，造粒机环模压缩比为1:(1.2～2.2)；
2)以70％～100％的丙酮作为提取剂对上述万寿菊花颗粒进行提取，过滤，得提取液；
3)下调提取液中丙酮的体积分数至0～30％，过滤，得滤饼，滤饼烘干得到万寿菊黄酮产品。
为了对上述技术方案更好的说明，进一步明确以下概念：
步骤1)所述的万寿菊花原料为新鲜或干燥的万寿菊花，或各类市场上可获得的万寿菊花的加工形式，例如花粕；步骤2)所述70％～100％丙酮是指丙酮的体积分数为70％～100％。
本发明技术方案中的技术参数可进一步作出如下选择：
步骤1)中造粒后颗粒硬度为3～8kg/cm 2；
步骤2)中提取温度为40～60℃；优选45-55℃；进一步优选50～55℃；
步骤2)中万寿菊花颗粒和提取溶剂的质量/体积(g/mL)比不小于1:2；优选1：(2～6)；进一步优选1：(3～5)；再进一步优选1:4；
步骤2)中的提取方式优选逆流萃取；
步骤2)中提取次数不少于4次；优选4～7次。
步骤2)中每次提取时间为0.5～2.5小时，优选1～2小时；进一步优选1.5小时。
步骤2)中丙酮的体积分数优选70-75％；或70-80％；或70-85％，或70-90％；或70-95％；或70％～100％；或75-80％；或75-85％；或75-90％；或75-95％；或75-100％；或80-85％；或80-90％；或80-95％；或80-100％；或85％-90％；或85％-95％；或85％～100％；或90-100％；或92-99％；或70％～99％；或75％～99％；或80％～99％；或85％～99％；或90％～99％。
本发明优选的一种连续提取高含量万寿菊黄酮的工业化方法，包括以下步骤：
1)使用造粒机对万寿菊花原料进行造粒，造粒机环模压缩比为1:(1.2～2.2)，造粒后颗粒硬度为3～8kg/cm；
2)以70％～100％的丙酮作为提取剂对上述万寿菊花颗粒进行逆流萃取，万寿菊花颗粒和提取溶剂的质量/体积(g/mL)比不小于1:2；提取温度为40～60℃，提取次数不少于4次；每次提取时间为0.5～2.5小时；过滤，得提取液；
3)下调提取液中丙酮的体积分数至0～30％，过滤，得滤饼，滤饼烘干得到万寿菊黄酮产品。
本申请连续提取高含量万寿菊黄酮的工业化方法，步骤3)中所述的下调提取液中有机溶剂体积分数的方式可以是浓缩或加入强极性溶剂。
本发明还提供了一种上述制备工艺制备获得的万寿菊黄酮产物。该产物中黄酮含量不低于98％。
本发明的有益效果：
1.本方法通过优化万寿菊花原料的预处理阶段，对原料进行造粒，优化造粒机环模压缩比，为规模化提取高含量万寿菊黄酮创造前提条件，同时发现控制造粒机环模压缩比对于万寿菊黄酮的特异提取具有很好的效果；
2.本方法通过控制的萃取溶剂以及提取液中有机溶剂的体积分数，实现对菊花中黄酮进行充分萃取的同时；还能使万寿菊黄酮与杂质实现很好的分离；
3.本发明的方法获得的万寿菊黄酮产品中黄酮含量≥98％，并能够实现生产连续，产能高、操作简单，满足工业化大生产的要求，实现高含量万寿菊黄酮产品的产业化，提高产业效益。
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。
各实施例中所使用的产品原料、试剂的规格均相同，所使用的造粒机、提取设备、过滤设备等均为相同设备。
实施例1
1)使用造粒机对万寿菊花粕进行造粒，造粒机的环模压缩比调整为1:1.8，通入蒸汽进行造粒；
2)万寿菊颗粒100kg，加入0.4m3的98％的丙酮，提取4次，每次1小时，提取液温度52℃左右；
3)提取液浓缩至丙酮的体积分数在10％左右；
4)过滤获得滤液和滤饼；
5)滤饼运输至烘干机进行烘干，获得实施例1产品。
实施例2
与实施例1相比，其区别在于，所述步骤1)环模压缩比1:1.2，其他操作与实施例1相同，获得实施例2产品。
实施例3
与实施例1相比，其区别在于，所述步骤1)环模压缩比1:2.2，其 他操作与实施例1相同，获得实施例3产品。
实施例4
与实施例1相比，其区别在于，所述步骤2)中采用92％丙酮对万寿菊颗粒进行提取，其他操作与实施例1相同，获得实施例4产品。
实施例5
与实施例1相比，其区别在于，所述步骤2)中采用70％丙酮对万寿菊颗粒进行提取，其他操作与实施例1相同，获得实施例5产品。
实施例6
与实施例1相比，其区别在于，所述步骤2)中采用100％丙酮对万寿菊颗粒进行提取，其他操作与实施例1相同，获得实施例6产品。
实施例7
与实施例1相比，其区别在于，所述步骤3)浓缩至丙酮体积分数为30％，其他操作与实施例1相同，获得实施例7产品。
实施例8
与实施例1相比，其区别在于，所述步骤3)浓缩至丙酮体积分数为0％(即浓缩至溶液中不含丙酮)，其他操作与实施例1相同，获得实施例8产品。
实施例9
与实施例1相比，其区别在于，所述步骤3)加入水溶液，调节至丙酮体积分数为10％，其他操作与实施例1相同，获得实施例9产品。
对比例1
与实施例1相比，其区别在于，所述步骤1)环模压缩比1:3.0，其他操作与实施例1相同，获得对比例1产品。
对比例2
与实施例1相比，其区别在于，所述步骤2)中采用浓度为65％丙酮对万寿菊颗粒进行提取，其他操作与实施例1相同，获得对比例2产品。
对比例3
与实施例1相比，其区别在于，所述步骤3)浓缩至丙酮体积分数为40％，其他操作与实施例1相同，获得对比例3产品。
对比例4
与实施例1相比，其区别在于，所述步骤3)中提取后不调节溶剂，直接浓缩并干燥，获得对比例4产品。
上述实施例及对比例获得的产品的含量及收率见下表：
表1万寿菊含量及收率表
产品 万寿黄酮含量 收率
实施例1 99.67％ 98.45％
实施例2 98.54％ 97.37％
实施例3 98.13％ 96.12％
实施例4 99.17％ 96.53％
实施例5 92.34％ 96.32％
实施例6 99.70％ 95.42％
实施例7 98.90％ 95.60％
实施例8 95.34％ 98.10％
实施例9 99.30％ 98.20％
对比例1 81.12％ 85.10％
对比例2 78.92％ 81.30％
对比例3 89.51％ 97.70％
对比例4 60.54％ 98.30％
上述万寿菊黄酮含量测定方法为：
将实施例及对比例制备获得的万寿菊黄酮样品利用乙醇溶解定容，加5％亚硝酸钠溶液1ml，摇匀，放置6min，加10％硝酸铝溶液1ml，摇匀，放置6min，加氢氧化钠试液10ml，再加水至刻度，摇匀，放置15min，以相应试剂为空白，按照紫外-可见分光光度法，在500nm的波长处测定 吸光度。以槲皮万寿菊素为标准对照品，进行含量计算。
收率技术方法为：
万寿菊黄酮收率(％)＝(产品总重×产品检测含量)×100％/(原料总重×原料检测含量)
上述含量及收率结果表明：造粒参数、提取前后溶剂中丙酮的含量，对万寿菊黄酮产品的提取效果具有明显的影响。本申请通过特定选择的造粒参数，以及提取前后溶剂中丙酮的含量，获得了最优的提取产品，取得了预料不到的技术效果。
以上内容是结合优选技术方案对本发明所做的进一步说明，所描述的实例是本发明的一部分实例，而不是全部实例。对于本发明所属技术领域的研究人员来说，在不脱离构思的前提下还可以做出简单推演和替换，在没有做出创造性劳动前提下所获得的其他实例，都属于本发明保护的范围。
工业实用性
本发明提供一种连续提取高含量万寿菊黄酮的工业化方法，其包括如下步骤：1)将万寿菊花原料进行造粒，造粒机环模压缩比为1:(1.2-2.2)；2)以70％～100％的丙酮作为提取剂对上述万寿菊花颗粒进行提取，过滤，得提取液；3)下调丙酮的体积分数在0～30％，过滤，得滤饼，滤饼烘干得到万寿菊黄酮产品。本发明方法简单，连续性、可操作性强，产能高、能耗少，适合工业化生产，具有较好的经济价值和应用前景。

Claims (9)

  1. 一种连续提取高含量万寿菊黄酮的工业化方法，其包括如下步骤：
    1)使用造粒机对万寿菊花原料进行造粒，造粒机环模压缩比为1:(1.2～2.2)；
    2)以70％～100％的丙酮作为提取剂对上述万寿菊花颗粒进行提取，过滤，得提取液；
    3)下调提取液中丙酮的体积分数至0～30％，过滤，得滤饼，滤饼烘干得到万寿菊黄酮产品。
  2. 根据权利要求1所述一种连续提取高含量万寿菊黄酮的工业化方法，其特征在于，所述1)中的万寿菊花原料为新鲜或干燥的万寿菊花,或各类市场上可获得的万寿菊花的加工形式；优选花粕。
  3. 根据权利要求1或2所述一种连续提取高含量万寿菊黄酮的工业化方法，其特征在于，步骤1)中造粒后颗粒硬度为3～8kg/cm 2。
  4. 根据权利要求1-3任一项所述一种连续提取高含量万寿菊黄酮的工业化方法，其特征在于，步骤2)中萃取温度为40～60℃。
  5. 根据权利要求1-4任一项所述一种连续提取高含量万寿菊黄酮的工业化方法，其特征在于，步骤2)中萃取颗粒和提取溶剂比不大于1：2(g/mL)。
  6. 根据权利要求1-5任一项所述一种连续提取高含量万寿菊黄酮的工业化方法，其特征在于，步骤2)中所述提取为逆流萃取。
  7. 根据权利要求1-6任一项所述一种连续提取高含量万寿菊黄酮的工业化方法，其特征在于，步骤2)中提取次数不少于4次；每次提取时间为0.5-2.5小时。
  8. 根据权利要求1-7任一项所述一种连续提取高含量万寿菊黄酮的工业方法，其特征在于，步骤2)中所述的下调溶剂体积分数的方式是浓缩或加入强极性溶剂。
  9. 一种如权利要求1-8任一项所述方法制备得到的万寿菊黄酮产品。
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