WO2023227138A1 - 从文冠木中提取杨梅素的方法 - Google Patents

从文冠木中提取杨梅素的方法 Download PDF

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WO2023227138A1
WO2023227138A1 PCT/CN2023/102795 CN2023102795W WO2023227138A1 WO 2023227138 A1 WO2023227138 A1 WO 2023227138A1 CN 2023102795 W CN2023102795 W CN 2023102795W WO 2023227138 A1 WO2023227138 A1 WO 2023227138A1
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myricetin
mixture
extracting
filter residue
extraction
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PCT/CN2023/102795
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English (en)
French (fr)
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李维佳
郑静美
闫婧怡
王军华
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河北瑞龙生物科技有限公司
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Priority to US18/478,522 priority Critical patent/US11944599B2/en
Priority to ZA2023/09465A priority patent/ZA202309465B/en
Publication of WO2023227138A1 publication Critical patent/WO2023227138A1/zh

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/33—Heterocyclic compounds
    • A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
    • A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
    • A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline 
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
    • C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
    • 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)
    • A61K36/77—Sapindaceae (Soapberry family), e.g. lychee or soapberry
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/40—Separation, e.g. from natural material; Purification
    • 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
    • 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
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Definitions

  • This application relates to the technical field of extracting active ingredients of traditional Chinese medicine, specifically, to a method for extracting myricetin from A. globula.
  • Brassica elegans belongs to the Sapindaceae family, and is also known as Brassica elegans, papaya, papaya, and Wendan leather. Its wood and branches and leaves are used for medicinal purposes. It is mostly distributed in Northeast China, North China, Northwest China and other places. It tastes slightly sweet, astringent, and It is bitter and has the effects of reducing swelling, relieving pain, and removing dampness. It can be used clinically to treat rheumatoid arthritis, rheumatic internal heat, leprosy, etc. Bronchocarpa contains flavonoids, coumarins and glycosides. The flavonoids included include: dihydromyricetin, myricetin, quercetin, rutin, dihydroquercetin, and sorbitol. and catechins.
  • Myricetin also known as myricetin, myricetin, myricetin, etc.
  • myricetin is a polyhydroxy flavonol compound that is easily soluble in organic solvents such as methanol, ethanol, acetone, and ethyl acetate. When administered in large doses, it has the effects of dispelling wind and removing dampness, warming menstruation and relieving pain, activating blood circulation and unblocking meridians.
  • the preparation method of myricetin is mainly through solvent extraction from natural vine tea and Vitaceae plants of the genus Vitaceae. Since the extraction process is susceptible to interference from other components, especially dihydromyricetin, resulting in the formation of myricetin. The extraction rate and purity of myricetin are low. Therefore, there is an urgent need to develop a preparation method for myricetin with high extraction rate and high purity.
  • This application proposes a method for extracting myricetin from B. esculenta to solve the problems of low myricetin extraction rate and low purity in the prior art.
  • the method for extracting myricetin from A. elata includes the following steps:
  • step S4 Combine the extract obtained in step S3 and the filtrate obtained in step S2 to obtain a second mixture, add an alkaline auxiliary agent to the second mixture to obtain a third mixture, and adjust the concentration of the third mixture.
  • the pH reaches 8 to 9. After heating and boiling, it is lowered to room temperature and concentrated under reduced pressure to obtain a concentrated solution;
  • the baking temperature in step S1 is 80°C to 100°C.
  • the moisture content of the coarse powder of A. striata in step S1 is ⁇ 2% (mass fraction).
  • the mass ratio of the A. estriata coarse powder and the countercurrent leaching liquid in the step S2 is 1:100-500.
  • the countercurrent leach liquid in step S2 is composed of a mixture of sucrose fatty acid ester (sucrose ester), Vietnamese red oil and ethanol with a mass ratio of 4:1:500 to 1000.
  • the temperature of low-temperature countercurrent leaching in step S2 is 25°C to 35°C, and the time is 20min to 40min.
  • the solvent in step S3 is any one of alcohols and acetone.
  • the mass ratio of the filter residue to the solvent in step S3 is 1:5-20; when multiple heating reflux extractions are performed, the mass ratio of the filter residue to the solvent in each extraction It is 1:5 ⁇ 20.
  • the alkaline auxiliary agent in step S4 is saccharin sodium.
  • the monohydric alcohol aqueous solution in step S5 is a monohydric alcohol aqueous solution with a volume fraction of 45% to 65%.
  • countercurrent leaching is a continuous (or intermittent) reverse contact flow between the material to be leached and the leaching liquid, so that the active ingredients in the material to be leached are dissolved.
  • the material to be extracted is the medicinal material of A. elata.
  • the medicinal materials of A. elegans are first roasted, crushed and sieved to obtain a coarse powder of A. sorbifolia, and then the coarse powder of A. Countercurrent leaching is performed in the leaching solution to extract the myricetin.
  • This application uses a low-temperature countercurrent extraction method, using a mixture of sucrose esters, Turkish red oil and ethanol as the countercurrent leaching liquid. Since sucrose esters and Turkish red oil are added to the countercurrent leaching liquid, sucrose esters and Vietnamese red oil are also added to the countercurrent leaching liquid. The compatibility of red oil has a synergistic effect, so that the extracted myricetin has high purity, and the low-temperature countercurrent leaching method disclosed in this application has a high extraction rate.
  • This application adds sodium saccharin during the extraction process of myricetin to further convert dihydromyricetin into myricetin, thereby improving the extraction rate and purity of myricetin.
  • step S4 Combine the extract obtained in step S3 and the filtrate obtained in step S2, add saccharin sodium, adjust the pH of the mixture to 8, heat and boil, then lower to room temperature, and concentrate under reduced pressure to obtain a concentrated solution;
  • step S4 Combine the extract obtained in step S3 and the filtrate obtained in step S2, add saccharin sodium, adjust the pH of the mixture to 9, heat and boil, then lower to room temperature, and concentrate under reduced pressure to obtain a concentrated solution;
  • step S4 Combine the extract obtained in step S3 and the filtrate obtained in step S2, add saccharin sodium, adjust the pH of the mixture to 8, heat and boil, then lower to room temperature, and concentrate under reduced pressure to obtain a concentrated solution;
  • step S4 Combine the extract obtained in step S3 and the filtrate obtained in step S2, add saccharin sodium, adjust the pH of the mixture to 8, heat and boil, then lower to room temperature, and concentrate under reduced pressure to obtain a concentrated solution;
  • step S4 Combine the extract obtained in step S3 and the filtrate obtained in step S2, add saccharin sodium, adjust the pH of the mixture to 9, heat and boil, then lower to room temperature, and concentrate under reduced pressure to obtain a concentrated solution;
  • Example 3 The only difference from Example 3 is that the countercurrent leaching liquid in step S2 is ethanol, and the remaining steps and experimental parameters are the same as in Example 3. In Comparative Example 1, 4.3 g of myricetin solid was obtained.
  • Example 3 The only difference from Example 3 is that no sucrose ester is added to the countercurrent extraction liquid in step S2, that is, the countercurrent extraction liquid in Comparative Example 2 is a mixture of Turkish red oil and ethanol with a mass ratio of 1:1000. In Comparative Example 2, 4.9 g of myricetin solid was obtained.
  • Example 3 The only difference from Example 3 is that no Turkish red oil is added to the countercurrent extraction liquid in step S2, that is, the countercurrent extraction liquid in Comparative Example 3 is a mixture of sucrose ester and ethanol with a mass ratio of 4:1000. In Comparative Example 3, 5.1 g of myricetin solid was obtained.
  • step S4 is an equal amount of sodium bicarbonate, and 5.8g myricetin solid is obtained.
  • Examples 1 to 5 have high extraction rates and purity in extracting myricetin from B. esculenta .
  • Comparative Example 1 a single component of ethanol was used as the countercurrent extraction liquid, in Comparative Example 2, Turkish red oil and ethanol were used as the countercurrent extraction liquid, and in Comparative Example 3, sucrose ester and ethanol were used as the countercurrent extraction solvent, all of which resulted in poor extraction results. Poor, the extraction rate and purity of myricetin are not as good as those in the embodiment.
  • the compatibility of sucrose ester and Vietnamese red oil has synergy. The effect is to improve the extraction rate and purity of myricetin from Amaranthus striata.
  • Comparative Example 4 The only difference between Comparative Example 4 and Example 3 is that the alkaline auxiliary agent was replaced by sodium bicarbonate in equal amounts, resulting in the extraction rate and purity of myricetin in Comparative Example 4 being inferior to Example 3.

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Abstract

本申请涉及中药有效成分提取技术领域，提出了从文冠木中提取杨梅素的方法，包括以下步骤：S1、将文冠木药材烘烤，粉碎，过筛，得到文冠木粗粉；S2、将文冠木粗粉与逆流浸提液混合，进行低温逆流浸提，得到滤液和滤渣；S3、将滤渣与溶剂混合，加热回流提取1～3次，得到提取液；S4、合并提取液和S2中得到的滤液，加入碱性助剂，调节pH至8～9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；S5、将浓缩液用一元醇水溶液在大孔吸附树脂中分离洗脱，收集洗脱液，干燥，得到杨梅素固体。通过上述技术方案，解决了现有技术中杨梅素提取率低、纯度低的问题。

Description

从文冠木中提取杨梅素的方法
本专利申请要求于2022年08月31日提交的中国专利申请No.CN202211054260.8的优先权。在先申请的公开内容通过整体引用并入本申请。
技术领域
本申请涉及中药有效成分提取技术领域，具体的，涉及从文冠木中提取杨梅素的方法。
 背景技术
文冠木属无患子科，别名文冠果、土木瓜、木瓜、温旦革子，以木材及枝叶供药用，多分布于中国东北、华北、西北等地，味微甘、涩、苦，具有消肿止痛，祛湿等功效，临床上可用于治疗风湿性关节炎，风湿内热，麻风病等。文冠木中含有黄酮类化合物、香豆素及苷类化合物，其中所含黄酮类化合物包括：二氢杨梅素、杨梅素、槲皮素、芦丁、二氢槲皮素、文冠木素和儿茶精。
杨梅素又名杨梅树皮素、杨梅黄酮、杨梅酮等，是一种多羟基黄酮醇化合物，易溶于甲醇、乙醇、丙酮、乙酸乙酯等有机溶剂。大剂量给药时具有祛风除湿、温经止痛、活血通络等功效。目前，杨梅素的制备方法主要是在天然藤茶和葡萄科蛇葡萄属植物中通过溶剂进行提取，由于在提取过程中易受到其它成分的干扰，特别是二氢杨梅素的干扰，导致杨梅素的提取率和纯度较低，因此，迫切需要开发出一种高提取率、高纯度杨梅素的制备方法。
 技术问题
本申请提出从文冠木中提取杨梅素的方法，以解决现有技术中杨梅素提取率低、纯度低的问题。
 技术解决方案
本申请的技术方案如下：
从文冠木中提取杨梅素的方法，包括以下步骤：
S1、将文冠木药材烘烤，然后将烘烤后的文冠木药材粉碎，过筛，得到文冠木粗粉；
S2、将所述文冠木粗粉与逆流浸提液混合，进行低温逆流浸提，得到滤液和滤渣；
S3、将所述滤渣与溶剂混合得到第一混合物，对所述第一混合物加热回流提取1～3次，得到提取液；
S4、合并步骤S3中得到的所述提取液和步骤S2中得到的所述滤液得到第二混合物，向所述第二混合物中加入碱性助剂得到第三混合物，调节所述第三混合物的pH至8～9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将所述浓缩液用一元醇水溶液在大孔吸附树脂中分离洗脱，收集洗脱液，干燥所述洗脱液，得到杨梅素固体。
作为本申请的一个实施例，所述步骤S1中烘烤温度为80℃～100℃。
作为本申请的一个实施例，所述步骤S1中所述文冠木粗粉的含水量≤2％（质量分数）。
作为本申请的一个实施例，所述步骤S2中所述文冠木粗粉与所述逆流浸提液的质量比为1:100～500。
作为本申请的一个实施例，所述步骤S2中所述逆流浸提液由质量比为4:1:500～1000的蔗糖脂肪酸酯（蔗糖酯）、土耳其红油和乙醇混合组成。
作为本申请的一个实施例，所述步骤S2中低温逆流浸提的温度为25℃～35℃，时间为20min～40min。
作为本申请的一个实施例，所述步骤S3中所述溶剂为醇类、丙酮中的任一种。
作为本申请的一个实施例，所述步骤S3中所述滤渣与所述溶剂的质量比为1:5～20；当进行多次加热回流提取时，每次提取时的滤渣与溶剂的质量比为1:5～20。
作为本申请的一个实施例，所述步骤S4中所述碱性助剂为糖精钠。
作为本申请的一个实施例，所述步骤S5中所述一元醇水溶液为体积分数45％～65％的一元醇水溶液。
本领域技术人员知晓，逆流浸提是通过将被浸提物料与浸提液的连续（或间歇）逆向接触流动，使被浸提物料中的有效成分溶出。本申请中被浸提物料为文冠木药材，在进行逆流浸提前，首先对文冠木药材进行烘烤、粉碎、过筛处理，得到文冠木粗粉，然后将文冠木粗粉在浸提液中进行逆流浸提，提取出其中的杨梅素。
 有益效果
1、本申请采用低温逆流浸提法，将蔗糖酯、土耳其红油和乙醇的混合液作为逆流浸提液，由于在逆流浸提液中添加了蔗糖酯和土耳其红油，同时蔗糖酯和土耳其红油配伍使用，具有协同效应，使提取出的杨梅素具有高的纯度，且本申请公开的低温逆流浸提法具有高的提取率。
2、本申请通过在杨梅素的提取过程中加入糖精钠，将二氢杨梅素进一步转换为杨梅素，从而提高了杨梅素的提取率和纯度。
 本发明的实施方式
下面将结合本申请实施例，对本申请实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都涉及本申请保护的范围。
实施例1
S1、将1kg文冠木药材在80℃烘烤，烘烤至水分质量含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在25℃进行逆流浸提40min，得到滤液和滤渣，文冠木粗粉与逆流浸提液的质量比为1:500，逆流浸提液由质量比为4:1:500的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与乙醇混合，加热回流提取1次，得到提取液；滤渣与乙醇的质量比为1:5；
S4、合并步骤S3中得到的提取液和步骤S2中得到的滤液，加入糖精钠，调节混合液的pH至8，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将浓缩液用体积分数为45％的乙醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.8g杨梅素固体。
实施例2
S1、将1kg文冠木药材在85℃烘烤，烘烤至水分质量含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在30℃进行逆流浸提30min，得到滤液和滤渣，文冠木粗粉与逆流浸提液的质量比为1:300，逆流浸提液由质量比为4:1:700的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与乙醇混合，加热回流提取3次，得到提取液；每次提取时滤渣与乙醇的质量比为1:8；
S4、合并步骤S3中得到的提取液和步骤S2中得到的滤液，加入糖精钠，调节混合液的pH至9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将浓缩液用体积分数为50％的乙醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.6g杨梅素固体。
实施例3
S1、将1kg文冠木药材在90℃烘烤，烘烤至水分质量含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在35℃进行逆流浸提20min，得到滤液和滤渣，文冠木粗粉与逆流浸提液的质量比为1:100，逆流浸提液由质量比为4:1:1000的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与甲醇混合，加热回流提取2次，得到提取液；每次提取时滤渣与甲醇的质量比为1:10；
S4、合并步骤S3中得到的提取液和步骤S2中得到的滤液，加入糖精钠，调节混合液的pH至8，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将浓缩液用体积分数为60％的甲醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.2g杨梅素固体。
实施例4
S1、将1kg文冠木药材在100℃烘烤，烘烤至水分质量含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在30℃进行逆流浸提40min，得到滤液和滤渣，文冠木粗粉与逆流浸提液的质量比为1:400，逆流浸提液由质量比为4:1:900的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与丙酮混合，加热回流提取3次，得到提取液；每次提取时滤渣与丙酮的质量比为1:20；
S4、合并步骤S3中得到的提取液和步骤S2中得到的滤液，加入糖精钠，调节混合液的pH至8，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将浓缩液用体积分数为65％的甲醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.3g杨梅素固体。
实施例5
S1、将1kg文冠木药材在95℃烘烤，烘烤至水分质量含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在35℃进行逆流浸提40min，得到滤液和滤渣，文冠木粗粉与逆流浸提液的质量比为1:350，逆流浸提液由质量比为4:1:750的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与丙酮混合，加热回流提取1次，得到提取液；滤渣与丙酮的质量比为1:18；
S4、合并步骤S3中得到的提取液和步骤S2中得到的滤液，加入糖精钠，调节混合液的pH至9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将浓缩液用体积分数为50％的甲醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.5g杨梅素固体。
对比例1
与实施例3的区别仅在于步骤S2中逆流浸提液为乙醇，其余步骤和实验参数与实施例3相同。对比例1中得到4.3g杨梅素固体。
对比例2
与实施例3的区别仅在于步骤S2中逆流浸提液中不添加蔗糖酯，即对比例2中的逆流提取液为质量比1:1000的土耳其红油和乙醇混合而成。对比例2中得到4.9g杨梅素固体。
对比例3
与实施例3的区别仅在于步骤S2中逆流浸提液中不添加土耳其红油，即对比例3中的逆流提取液为质量比4:1000的蔗糖酯和乙醇混合而成。对比例3中得到5.1g杨梅素固体。
对比例4
与实施例3的区别仅在于步骤S4中碱性助剂为等量的碳酸氢钠，得到5.8g杨梅素固体。
提取率（%）＝(杨梅素固体的质量/文冠木药材的质量)×100％
将实施例1～5与对比例1～4制备的杨梅素固体采用高效液相色谱法(High Performance Liquid Chromatography, HPLC)测定杨梅素的纯度，高效液相色谱(HPLC)的各项实验参数均为本领域的常规技术手段，测试结果见表1。
表1杨梅素的提取率、纯度
由表1可以看出，实施例1～5从文冠木中提取杨梅素具有高的提取率和纯度。
而对比例1中使用单一组分的乙醇作为逆流浸提液，对比例2使用土耳其红油和乙醇作为逆流浸提液，对比例3使用蔗糖酯和乙醇作为逆流提取溶剂，均导致提取效果较差，杨梅素的提取率和纯度均不如实施例，同时，将对比例1～3与实施例3杨梅素的提取率和纯度对比后，发现蔗糖酯和土耳其红油二者配伍使用，具有协同效果，提高了从文冠木中提取杨梅素的提取率和纯度。
对比例4与实施例3的区别仅在于将碱性助剂等量替换为碳酸氢钠，导致对比例4杨梅素的提取率和纯度不如实施例3。
以上仅为本申请的较佳实施例而已，并不用以限制本申请，凡在本申请的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本申请的保护范围之内。

Claims (6)

  1. 从文冠木中提取杨梅素的方法，其特征在于，包括以下步骤：
    S1、将文冠木药材烘烤，然后将烘烤后的文冠木药材粉碎，过筛，得到文冠木粗粉；
    S2、将所述文冠木粗粉与逆流浸提液混合，进行低温逆流浸提，得到滤液和滤渣；
    S3、将所述滤渣与溶剂混合得到第一混合物，对所述第一混合物加热回流提取1~3次，得到提取液；
    S4、合并步骤S3中得到的所述提取液和步骤S2中得到的所述滤液得到第二混合物，向所述第二混合物中加入碱性助剂得到第三混合物，调节所述第三混合物的pH至8~9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
    S5、将所述浓缩液用一元醇水溶液在大孔吸附树脂中分离洗脱，收集洗脱液，干燥所述洗脱液，得到杨梅素固体；
    所述步骤S2中所述文冠木粗粉与所述逆流浸提液的质量比为1:100~500；
    所述步骤S2中所述逆流浸提液由质量比为4:1:500~1000的蔗糖酯、土耳其红油和乙醇混合组成；
    所述步骤S2中低温逆流浸提的温度为25℃~35℃，时间为20min~40min；
    所述步骤S4中所述碱性助剂为糖精钠。
  2. 根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述步骤S1中烘烤温度为80℃~100℃。
  3. 根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述步骤S1中所述文冠木粗粉的含水量≤2%。
  4. 根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述步骤S3中所述溶剂为醇类、丙酮中的任一种。
  5. 根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述步骤S3中所述滤渣与所述溶剂的质量比为1:5~20。
  6. 根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述步骤S5中所述一元醇水溶液为体积分数45%~65%的一元醇水溶液。
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