CN106038821A - Method for extracting total flavonoids from boxthorn leaves - Google Patents
Method for extracting total flavonoids from boxthorn leaves Download PDFInfo
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- 244000241838 Lycium barbarum Species 0.000 title claims abstract description 44
- 235000015459 Lycium barbarum Nutrition 0.000 title claims abstract description 44
- 229930003935 flavonoid Natural products 0.000 title claims abstract description 36
- 150000002215 flavonoids Chemical class 0.000 title claims abstract description 36
- 235000017173 flavonoids Nutrition 0.000 title claims abstract description 36
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- 238000000605 extraction Methods 0.000 claims abstract description 66
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- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
- A61K36/815—Lycium (desert-thorn)
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- A61K2236/30—Extraction of the material
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- 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
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Abstract
Description
技术领域technical field
本发明涉及一种从枸杞叶中提取总黄酮的方法，具体涉及利用高效回流浓缩提取-柱层析分离枸杞叶总黄酮的方法，属于天然药材的有效成分提取领域。The invention relates to a method for extracting total flavonoids from wolfberry leaves, in particular to a method for separating total flavonoids from wolfberry leaves by high-efficiency reflux concentration extraction-column chromatography, and belongs to the field of effective component extraction of natural medicinal materials.
背景技术Background technique
从植物中提取化学成分作为药用，在祖国传统医药学中已有5000年的历史。传统提取方法按照提取过程对能量需求方式的不同可以分为两大类。一类是加热提取法，主要有煎煮提取法、回流提取法和索氏提取法等不同方式；另一类是浸泡提取法，主要有浸渍提取法和渗漉提取法两种。传统提取法存在着提取时间长、工艺繁复、效率低、工业污染大和对目标化合物提取无选择性等缺陷。Extracting chemical components from plants for medicinal purposes has a history of 5,000 years in the traditional medicine of the motherland. Traditional extraction methods can be divided into two categories according to the different energy requirements of the extraction process. One is the heating extraction method, which mainly includes different methods such as decoction extraction, reflux extraction and Soxhlet extraction; the other is the soaking extraction method, which mainly includes dipping extraction and percolation extraction. Traditional extraction methods have disadvantages such as long extraction time, complicated process, low efficiency, large industrial pollution and no selectivity for the extraction of target compounds.
高效回流浓缩技术是药物动态提取，药物与溶剂间含溶质高梯度，增加了浸出推动力，增加了得膏率。可比常规法多提取5～20％以上。提取、浓缩一步完成，提取时间短，提取物药用成份质量提高。The high-efficiency reflux concentration technology is a dynamic extraction of drugs, with a high gradient of solute between the drug and the solvent, which increases the driving force of leaching and increases the yield of paste. It can extract more than 5-20% more than the conventional method. The extraction and concentration are completed in one step, the extraction time is short, and the quality of the medicinal components of the extract is improved.
枸杞叶又名“天精草”，枸杞叶(Lycium Chinese)俗称天精草，《本草纲目》中称枸杞叶“有除烦益志补五劳七伤，壮心气，除热毒，散疮肿，除风明目”之功效。枸杞总黄酮化合物(TFL Total Flavonoids of Lycium barbarum L.)是枸杞叶主要有效成分之一，含量达577mg/100g。黄酮化合物具有止咳、平喘、祛痰，并能扩张冠状动脉及降低血胆固醇，增强心脏收缩、减少心脏搏动数及清除自由基等作用。本专利中提取物黄酮化合物的含量及成分检测是采用高效液相色谱法(HPLC)检测。Lycium leaves are also known as "Tianjingcao". Lycium Chinese is commonly known as Tianjingcao. In "Compendium of Materia Medica", it is said that wolfberry leaves "can relieve annoyance, benefit will, five labors and seven injuries, strengthen the heart, remove heat and poison, and relieve sores. swelling, removing wind and improving eyesight". Lycium barbarum total flavonoids (TFL Total Flavonoids of Lycium barbarum L.) is one of the main active ingredients of Lycium barbarum leaves, with a content of 577mg/100g. Flavonoids have the functions of relieving cough, relieving asthma, eliminating phlegm, expanding coronary arteries, lowering blood cholesterol, enhancing cardiac contraction, reducing heart beat rate and scavenging free radicals. In this patent, the content and composition of the flavonoids in the extract are detected by high performance liquid chromatography (HPLC).
目前，从枸杞叶中提取枸杞叶总黄酮化合物的方法基本有三大类，水提取法、碱性水或碱性稀醇提取法、有机溶剂提取法、微波法、超声波法。水提取法工艺成本低，安全，但是提取效率低，含杂质多，给后续分离带来许多困难。碱性水或碱性稀醇提取法采用的碱性溶液是稀氢氧化钠和石灰水(氢氧化钙水溶液)，氢氧化钠水溶液的浸出能力高，但杂质较多不利于纯化，石灰水中的钙会与有些黄酮类化合物结合成不溶性物质，降低浸出率。微波法客服了上述方法中的一些缺陷，但提取过程中，微波的热效应会导致提取物中某些热命物质降解，严重影响提取物的活性，也限制了该方法的广泛应用。超声波法浸提时间短，效率高，但难以实现大规模工业化生产。本发明的目的在于克服现有技术中存在的缺点，采用高效回流浓缩提取设备，利用高效回流浓缩-柱层析提取纯化技术，提供从枸杞叶中快速、高效地获得枸杞叶总黄酮物质的新方法。即：提供一种可以取代上述工艺过程的简单易行、高效、快速、成本低，废液排放量少的新方法。At present, there are basically three types of methods for extracting total flavonoids from Lycium barbarum leaves, water extraction, alkaline water or alkaline dilute alcohol extraction, organic solvent extraction, microwave method, and ultrasonic method. The water extraction process is low in cost and safe, but the extraction efficiency is low and it contains many impurities, which brings many difficulties to the subsequent separation. The alkaline solution used in alkaline water or alkaline dilute alcohol extraction method is dilute sodium hydroxide and lime water (calcium hydroxide aqueous solution). The leaching ability of sodium hydroxide aqueous solution is high, but there are many impurities that are not conducive to purification. Calcium will combine with some flavonoids to form insoluble substances, reducing the leaching rate. The microwave method overcomes some defects in the above methods, but during the extraction process, the thermal effect of microwave will cause the degradation of some thermal substances in the extract, which seriously affects the activity of the extract, and also limits the wide application of this method. The ultrasonic extraction time is short and the efficiency is high, but it is difficult to realize large-scale industrial production. The purpose of the present invention is to overcome the shortcoming that exists in the prior art, adopt high-efficiency reflux concentration extraction equipment, utilize high-efficiency reflux concentration-column chromatography extraction and purification technology, provide the new method that obtains the total flavonoids of wolfberry leaves from wolfberry leaves quickly and efficiently method. Namely: to provide a new method that can replace the above-mentioned process, which is simple, efficient, fast, low in cost and less in waste liquid discharge.
发明内容Contents of the invention
本发明是采用正交试验设计方案，通过筛选提取过程中的溶剂类型、料液比、提取时间、提取温度等技术参数，获得快速、准确、高效、经济的从枸杞叶中提取黄酮类物质的方法。The present invention adopts an orthogonal experiment design scheme, and obtains a fast, accurate, efficient and economical method of extracting flavonoids from Lycium barbarum leaves by screening technical parameters such as solvent type, solid-liquid ratio, extraction time, and extraction temperature in the extraction process. method.
为达到上述目的，本发明的技术方案为：To achieve the above object, the technical solution of the present invention is:
一种从枸杞叶中提取总黄酮的方法，其特征在于，按下列步骤进行：A method for extracting total flavonoids from Lycium barbarum leaves, characterized in that, the following steps are carried out:
1.将枸杞叶粉碎至2-4mm粒径大小，70％乙醇溶剂高效回流提取浓缩，浸膏经石油醚萃取去除叶绿素等脂溶性色素，将萃取后的水液过大孔吸附树脂柱，该大孔树脂型号为D101，以纯水洗涤去除水溶性糖类物质，以30％-60％乙醇洗脱，收集洗脱液，将洗脱液回收乙醇，浓缩，减压干燥，得枸杞叶总黄酮提取物。1. Grind wolfberry leaves to a particle size of 2-4mm, extract and concentrate with high-efficiency reflux of 70% ethanol solvent, extract fat-soluble pigments such as chlorophyll through petroleum ether extraction, and pass the extracted water through a macroporous adsorption resin column. The macroporous resin model is D101, washed with pure water to remove water-soluble sugars, eluted with 30%-60% ethanol, collected the eluate, recovered ethanol from the eluate, concentrated, and dried under reduced pressure to obtain total leaves of Lycium barbarum. Flavonoid Extract.
2.进一步，所述的一种从枸杞叶中提取总黄酮的方法，其提取材料条件特征为10月采摘枸杞叶片，经60℃烘干，粉碎至2-4mm粒径。2. Further, the method for extracting total flavonoids from Lycium barbarum leaves is characterized in that the extraction material conditions are that the leaves of Lycium barbarum are picked in October, dried at 60°C, and crushed to a particle size of 2-4mm.
3.进一步，所述的一种从枸杞叶中提取总黄酮的方法，其提取方法条件特征为：采用高效回流浓缩提取设备，提取温度85℃，提取溶剂70％乙醇，料液比1∶12，提取时间1.5h。3. Further, the described method for extracting total flavonoids from Lycium barbarum leaves is characterized by the following conditions: high-efficiency reflux concentration extraction equipment, extraction temperature of 85°C, extraction solvent 70% ethanol, and a solid-liquid ratio of 1:12 , extraction time 1.5h.
4.进一步，所述的一种从枸杞叶中提取总黄酮的方法，上述样品用大孔吸附树脂柱层析，先用水洗脱，3-4倍柱体积除去可溶性糖及水溶性杂质，再用30～60％乙醇洗脱4～6个柱体积，收集洗脱液，60℃下浓缩、干燥即得产品。4. Further, in the described method of extracting total flavonoids from Lycium barbarum leaves, the above-mentioned sample is chromatographed on a macroporous adsorption resin column, and first washed with water, and 3-4 times column volume is used to remove soluble sugar and water-soluble impurities, and then Elute with 30-60% ethanol for 4-6 column volumes, collect the eluate, concentrate and dry at 60°C to obtain the product.
5.进一步，所述的一种从枸杞叶中提取总黄酮的方法，其提取效率特征为枸杞叶总黄酮提取率可达82.5％，所得产品经HPLC方法检测其中有效成分为芦丁、山奈酚、异鼠李素、槲皮素，含量分别为93.05％、3.31％、2.99％、0.65％。5. Further, the described method for extracting total flavonoids from Lycium barbarum leaves, its extraction efficiency is characterized by the extraction rate of total flavonoids from Lycium barbarum leaves can reach 82.5%, and the obtained product is detected by HPLC method wherein the active ingredients are rutin and kaempferol , isorhamnetin, and quercetin, the contents of which are 93.05%, 3.31%, 2.99%, and 0.65%, respectively.
本发明采用高效回流浓缩提取-柱层析纯化技术从枸杞叶中提取黄酮类物质的方法与已有提取技术相比，具有以下优点和显著效果：Compared with the existing extraction technology, the method for extracting flavonoids from Lycium barbarum leaves by adopting high-efficiency reflux concentration extraction-column chromatography purification technology has the following advantages and significant effects:
①缩短提取浓缩时间：高效回流浓缩提取可实现提取-浓缩同步完成，提取时间较传统方法可缩短6-8倍以上，浸膏得率较常规法提高5～20％，提高了设备处理量和效率。①Shorten the extraction and concentration time: high-efficiency reflux concentration extraction can realize extraction-concentration synchronously, the extraction time can be shortened by more than 6-8 times compared with the traditional method, and the extract yield is increased by 5-20% compared with the conventional method, which improves the equipment processing capacity and efficiency.
②操作简便，条件易控，节约溶媒，节省时间，降低能耗，设备维护保养方便，易于大规模工业化生产。②The operation is simple, the conditions are easy to control, the solvent is saved, the time is saved, the energy consumption is reduced, the maintenance of the equipment is convenient, and it is easy for large-scale industrial production.
具体实施方式detailed description
以下为本发明较佳的实施方式，并不因此而限定了本发明的保护范围。The following are preferred embodiments of the present invention, which do not limit the protection scope of the present invention.
一种从枸杞叶中提取总黄酮的方法，按下列步骤进行：A method for extracting total flavonoids from Lycium barbarum leaves, carried out according to the following steps:
1.将枸杞叶粉碎至2-4mm粒径大小，70％乙醇溶剂高效回流提取浓缩，浸膏经石油醚萃取去除叶绿素等脂溶性色素，将萃取后的水液过大孔吸附树脂柱，该大孔树脂型号为D101，以纯水洗涤去除水溶性糖类物质，以30％-60％乙醇洗脱，收集洗脱液，将洗脱液回收乙醇，浓缩，减压干燥，得枸杞叶总黄酮提取物。1. Grind wolfberry leaves to a particle size of 2-4mm, extract and concentrate with high-efficiency reflux of 70% ethanol solvent, extract fat-soluble pigments such as chlorophyll through petroleum ether extraction, and pass the extracted water through a macroporous adsorption resin column. The macroporous resin model is D101, washed with pure water to remove water-soluble sugars, eluted with 30%-60% ethanol, collected the eluate, recovered ethanol from the eluate, concentrated, and dried under reduced pressure to obtain total leaves of Lycium barbarum. Flavonoid Extract.
2.进一步，所述的一种从枸杞叶中提取总黄酮的方法，其提取材料条件特征为10月采摘枸杞叶片，经60℃烘干，粉碎至2-4mm粒径。2. Further, the method for extracting total flavonoids from Lycium barbarum leaves is characterized in that the extraction material conditions are that the leaves of Lycium barbarum are picked in October, dried at 60°C, and crushed to a particle size of 2-4mm.
3.进一步，所述的一种从枸杞叶中提取总黄酮的方法，其提取方法条件特征为：采用高效回流浓缩提取设备，提取温度85℃，提取溶剂70％乙醇，料液比1∶12，提取时间1.5h。3. Further, the described method for extracting total flavonoids from Lycium barbarum leaves is characterized by the following conditions: high-efficiency reflux concentration extraction equipment, extraction temperature of 85°C, extraction solvent 70% ethanol, and a solid-liquid ratio of 1:12 , extraction time 1.5h.
4.进一步，所述的一种从枸杞叶中提取总黄酮的方法，上述样品用大孔吸附树脂柱层析，先用水洗脱，3-4倍柱体积除去可溶性糖及水溶性杂质，再用30～60％乙醇洗脱4～6个柱体积，收集洗脱液，60℃下浓缩、干燥即得产品。4. Further, in the described method of extracting total flavonoids from Lycium barbarum leaves, the above-mentioned sample is chromatographed on a macroporous adsorption resin column, and first washed with water, and 3-4 times column volume is used to remove soluble sugar and water-soluble impurities, and then Elute with 30-60% ethanol for 4-6 column volumes, collect the eluate, concentrate and dry at 60°C to obtain the product.
5.进一步，所述的一种从枸杞叶中提取总黄酮的方法，其提取效率特征为枸杞叶总黄酮提取率可达82.5％，所得产品经HPLC方法检测其中有效成分为芦丁、山奈酚、异鼠李素、槲皮素，含量分别为93.05％、3.31％、2.99％、0.65％。5. Further, the described method for extracting total flavonoids from Lycium barbarum leaves, its extraction efficiency is characterized by the extraction rate of total flavonoids from Lycium barbarum leaves can reach 82.5%, and the obtained product is detected by HPLC method wherein the active ingredients are rutin and kaempferol , isorhamnetin, and quercetin, the contents of which are 93.05%, 3.31%, 2.99%, and 0.65%, respectively.
实施例1：Example 1:
以10月采摘的枸杞叶片，经60℃烘干，粉碎，粒径2-4mm为材料。投入萃取斧中加入70％乙醇，料液比(kg∶L)1∶10，混合；提取温度：85℃，总提取时间1.5h；依上述方法，枸杞叶黄酮提取率可达82.5％。Lycium barbarum leaves picked in October are dried at 60°C, crushed, and the particle size is 2-4 mm. Add 70% ethanol to the extraction axe, the ratio of solid to liquid (kg:L) is 1:10, and mix; extraction temperature: 85°C, total extraction time 1.5h; according to the above method, the extraction rate of flavonoids from wolfberry leaves can reach 82.5%.
本发明采用高效回流浓缩提取-柱层析纯化技术从枸杞叶中提取黄酮类物质的方法与已有提取技术相比，具有以下优点和显著效果：高效回流浓缩提取可实现提取-浓缩同步完成，提取时间较传统方法可缩短6-8倍以上，浸膏得率较常规法提高5～20％，提高了设备处理量和效率；操作简便，条件易控，节约溶媒，节省时间，降低能耗，设备维护保养方便，易于大规模工业化生产。Compared with the existing extraction technology, the method for extracting flavonoids from Lycium barbarum leaves by adopting high-efficiency reflux concentration extraction-column chromatography purification technology has the following advantages and significant effects: high-efficiency reflux concentration extraction can realize extraction-concentration synchronously, The extraction time can be shortened by more than 6-8 times compared with the traditional method, and the extraction rate of the extract is increased by 5-20% compared with the conventional method, which improves the processing capacity and efficiency of the equipment; the operation is simple, the conditions are easy to control, the solvent is saved, the time is saved, and the energy consumption is reduced , The equipment is easy to maintain and easy to mass industrial production.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107898868A (en) * | 2017-10-24 | 2018-04-13 | 中国科学院兰州化学物理研究所 | The method that separated in synchronization prepares matrimony vine red pigment, polysaccharides and matrimony vine flavones from matrimony vine |
| CN108159187A (en) * | 2018-01-22 | 2018-06-15 | 周学义 | A kind of method that flavones is extracted from wolfberry leaf |
| NL2028620B1 (en) * | 2021-07-02 | 2022-06-16 | Wolfberry Science Inst Ningxia Academy Of Agriculture And Forestry Sciences | Method for extracting total flavonoids from lycium chinese leaves |
| CN115812961A (en) * | 2022-11-16 | 2023-03-21 | 天津科技大学 | Application of total polyphenol of medlar in preparing food for regulating intestinal flora |
| CN118903296A (en) * | 2024-09-06 | 2024-11-08 | 中国科学院兰州化学物理研究所 | Method for preparing extract for preventing and treating nonalcoholic steatohepatitis from Lycii folium |
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2016
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Non-Patent Citations (1)
| Title |
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| 刘兰英等: "枸杞叶黄酮纯化工艺研究", 《食品科学》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107898868A (en) * | 2017-10-24 | 2018-04-13 | 中国科学院兰州化学物理研究所 | The method that separated in synchronization prepares matrimony vine red pigment, polysaccharides and matrimony vine flavones from matrimony vine |
| CN108159187A (en) * | 2018-01-22 | 2018-06-15 | 周学义 | A kind of method that flavones is extracted from wolfberry leaf |
| NL2028620B1 (en) * | 2021-07-02 | 2022-06-16 | Wolfberry Science Inst Ningxia Academy Of Agriculture And Forestry Sciences | Method for extracting total flavonoids from lycium chinese leaves |
| CN115812961A (en) * | 2022-11-16 | 2023-03-21 | 天津科技大学 | Application of total polyphenol of medlar in preparing food for regulating intestinal flora |
| CN118903296A (en) * | 2024-09-06 | 2024-11-08 | 中国科学院兰州化学物理研究所 | Method for preparing extract for preventing and treating nonalcoholic steatohepatitis from Lycii folium |
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