CN101412703A - Composite extracting technique for coproduction of mulberry tea flavone, polysaccharide and alkaloid - Google Patents
Composite extracting technique for coproduction of mulberry tea flavone, polysaccharide and alkaloid Download PDFInfo
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Abstract
Description
一、技术领域 1. Technical field
本发明属于生物分离技术领域，特别涉及一种联产桑叶黄酮、多糖和生物碱的复合提取工艺。The invention belongs to the technical field of biological separation, and in particular relates to a composite extraction process for co-producing flavonoids, polysaccharides and alkaloids of mulberry leaves.
二、背景技术 2. Background technology
现有技术：桑叶为桑科植物桑(Morus alba L.)的干燥叶，性寒，味甘苦，具有疏散风热、清肺润燥、清肝明目等功效，是常用中药之一，主要用于外感风热所致的发热、头昏头痛、咳嗽、咽喉肿痛等症，还用于肝经实热所致的目赤、涩痛、多泪等症。桑叶营养丰富，含有人体所需的16种氨基酸，7种维生素还含有钙、铁、锌、锰等营养元素，具有药性平和、无毒副作用等特点。桑叶的药用在我国历史悠久，将其作为天然药物加以应用非常广泛。《神农本草经》称桑叶为“神仙叶”，具有滋阴补血，疏散风热，益肝通气，降压利尿之功效。《本草纲目》记载：桑叶乃手足阳明之药，汁煎代茗，能止消渴，明目长发。《寿世保元》中以桑叶为主的扶桑至宝丹“久服不以自登上寿”。Prior art: Mulberry leaf is the dry leaf of Moraceae plant Morus (Morus alba L.), cold in nature, sweet and bitter in taste, has the effects of dispelling wind-heat, clearing lung and moistening dryness, clearing liver and improving eyesight, and is one of the commonly used traditional Chinese medicines. It is mainly used for symptoms such as fever, dizziness, headache, cough, and sore throat caused by exogenous wind-heat, and it is also used for symptoms such as red eyes, astringent pain, and excessive tears caused by excess heat in the liver meridian. Mulberry leaves are rich in nutrients, containing 16 kinds of amino acids needed by the human body, and 7 kinds of vitamins also contain nutrients such as calcium, iron, zinc, manganese, etc., and have the characteristics of mild medicinal properties and no toxic side effects. The medicinal use of mulberry leaves has a long history in my country, and it is widely used as a natural medicine. "Shen Nong's Materia Medica" calls mulberry leaves "immortal leaves", which have the effects of nourishing yin and blood, dispelling wind and heat, benefiting liver and ventilating, and reducing blood pressure and diuresis. "Compendium of Materia Medica" records: Mulberry leaves are a medicine for the Yangming of the hands and feet, and the juice is fried instead of tea, which can relieve thirst, improve eyesight and grow hair. In "Shou Shi Bao Yuan", the mulberry leaf-based Fusang Zhibaodan "is not used for a long time to ascend the longevity".
我国是桑树的起源中心，桑属植物有15个种4个变种，因此桑树的种质类型丰富多样。我国大部分地区均有桑树分布与栽培，全国桑园面积约1000万亩，其中以江苏、浙江、四川等主产区产量最多。桑叶是桑树生物产量最大的部分，在实际蚕桑生产中，往往出现桑叶过剩的情况，这造成资源的极大浪费。若对这些资源加以充分利用，其经济效益与社会效益均相当可观。现代药理研究发现，桑叶提取物在治疗糖尿病、高血压、高血脂等症及抗衰老、抗病毒、抗炎等方面都具有良好的疗效，这与桑叶中的黄酮、多糖和生物碱等有效成分密切相关，其中桑叶黄酮的药理活性最为显著。因此，近年来人们已经开始越来越多地关注到桑叶黄酮、多糖和生物碱等药用成分资源的综合利用与开发。my country is the origin center of mulberry trees. There are 15 species and 4 varieties of Morus genus, so the germplasm types of mulberry trees are rich and diverse. Mulberry trees are distributed and cultivated in most areas of my country. The area of mulberry gardens in the country is about 10 million mu, of which Jiangsu, Zhejiang, Sichuan and other major producing areas have the largest output. Mulberry leaves are the part with the largest biological yield of mulberry trees. In actual sericulture production, there is often a surplus of mulberry leaves, which causes a great waste of resources. If these resources are fully utilized, their economic and social benefits are considerable. Modern pharmacological research has found that mulberry leaf extract has good curative effects in the treatment of diabetes, high blood pressure, hyperlipidemia and other diseases, as well as anti-aging, anti-virus, anti-inflammatory, etc., which is similar to the flavonoids, polysaccharides and alkaloids in mulberry leaves. The active ingredients are closely related, and the pharmacological activity of mulberry leaf flavonoids is the most significant. Therefore, in recent years, people have begun to pay more and more attention to the comprehensive utilization and development of medicinal ingredients resources such as mulberry leaf flavonoids, polysaccharides and alkaloids.
目前，有关桑叶中有效成分的提取方法已经有一些相关专利报道，如CN1683360公开了分别采用乙醇和水为提取剂和洗脱剂，利用大孔吸附树脂提取分离桑叶黄酮的方法，CN1351085公开了一种从桑叶中提取分子量在15000-50000道尔顿之间的桑叶多糖组分的方法，CN1338275公开了从桑叶中提取具有α-糖苷酶抑制剂活性的桑叶总生物碱的制备方法，CN1762428公开了利用超临界CO2从桑叶中萃取脱氧野尻酶素类生物碱和黄酮两种有效成分的方法，CN1850166公开了从桑叶中制备多糖和生物碱的分离方法并以此制备了桑叶降血糖有效组分组合物，CN1589835公开了含有桑叶黄酮、桑叶多酚、桑叶多糖、DNJ、GABA等多种生物活性成分的桑叶提取物及其用途。以上专利对桑叶有效部位提取工艺大多是针对单一的黄酮或多糖或生物碱，或其中的两种有效部位，未见以桑叶黄酮、多糖及生物碱三者为目标的复合提取工艺，没有实现联产桑叶黄酮、多糖及生物碱三种药用成分，极大的浪费了宝贵的桑叶资源。At present, there have been some related patent reports on the extraction method of active ingredients in mulberry leaves. For example, CN1683360 discloses the method of using ethanol and water as extractant and eluent respectively, and utilizes macroporous adsorption resin to extract and separate mulberry leaf flavonoids. CN1351085 discloses A method for extracting mulberry leaf polysaccharide components with a molecular weight between 15000-50000 Daltons from mulberry leaves, CN1338275 discloses the method of extracting mulberry leaf total alkaloids with α-glucosidase inhibitor activity from mulberry leaves Preparation method, CN1762428 discloses utilizing supercritical CO from mulberry leaves to extract deoxynojirizyme alkaloids and flavonoids two active ingredients method, CN1850166 discloses the separation method of preparing polysaccharide and alkaloids from mulberry leaves and uses this A composition of effective components of mulberry leaves for lowering blood sugar is prepared. CN1589835 discloses mulberry leaf extracts containing various bioactive components such as mulberry leaf flavonoids, mulberry leaf polyphenols, mulberry leaf polysaccharides, DNJ, GABA, and the use thereof. Most of the above patents on the extraction process of the effective parts of mulberry leaves are aimed at a single flavonoid or polysaccharide or alkaloid, or two effective parts thereof. The realization of co-production of three medicinal components of mulberry leaf flavonoids, polysaccharides and alkaloids greatly wastes precious mulberry leaf resources.
虽然现有技术表明桑叶中的黄酮、多糖及生物碱等单一的活性物质都有相关的提取工艺，但未从综合利用药用成分资源的角度深度开发桑叶资源，未形成一套提取桑叶中典型三大活性物质的复合工艺，对复合提取桑叶中的黄酮、多糖及生物碱的应用研究缺乏基础数据。因而，开发联产桑叶黄酮、多糖及生物碱的复合提取工艺制备相应的提取物，适于工业化生产，为其在医药、保健、食品、化妆品等工业上开拓新市场具有十分重要的意义。Although the prior art shows that single active substances such as flavonoids, polysaccharides and alkaloids in mulberry leaves have relevant extraction processes, they have not developed mulberry leaf resources in depth from the perspective of comprehensive utilization of medicinal ingredient resources, and have not formed a set of methods for extracting mulberry leaves. The composite process of the three typical active substances in the leaves lacks basic data for the application research of the composite extraction of flavonoids, polysaccharides and alkaloids in mulberry leaves. Therefore, it is of great significance to develop a compound extraction process for the co-production of mulberry leaf flavonoids, polysaccharides and alkaloids to prepare corresponding extracts, which is suitable for industrial production and is of great significance for opening up new markets in industries such as medicine, health care, food, and cosmetics.
三、发明内容 3. Contents of the invention
技术问题：本发明针对上述技术空白，提供一种联产桑叶黄酮、多糖和生物碱的复合提取工艺。该方法可以适用于多种桑叶资源中三种有效组分的提取分离，实现桑叶资源的高值化多组分综合利用。Technical problem: The present invention aims at the above-mentioned technical blank, and provides a composite extraction process for the co-production of mulberry leaf flavonoids, polysaccharides and alkaloids. The method can be applied to the extraction and separation of three effective components in various mulberry leaf resources, and realizes the high-value multi-component comprehensive utilization of mulberry leaf resources.
技术方案：一种联产桑叶黄酮、多糖和生物碱的复合提取工艺，提取步骤为：Technical solution: a composite extraction process for co-production of mulberry leaf flavonoids, polysaccharides and alkaloids, the extraction steps are:
a.原料处理：以新鲜桑叶为原料，烘干变脆后，粉碎过筛得桑叶粉；a. Raw material processing: take fresh mulberry leaves as raw materials, after drying and becoming brittle, crush and sieve to obtain mulberry leaf powder;
b.提取：将桑叶粉用水浸提后过滤，得桑叶残渣和桑叶水提液，将桑叶残渣加入盐酸-乙醇-水溶液提取获得含桑叶生物碱的溶液；b. Extraction: extract the mulberry leaf powder with water and filter to obtain the mulberry leaf residue and mulberry leaf water extract, add the mulberry leaf residue to hydrochloric acid-ethanol-water solution for extraction to obtain a solution containing mulberry leaf alkaloids;
c.分离：将所得桑叶水提液通过大孔吸附树脂柱进行吸附后，先用蒸馏水洗脱树脂柱至无色，得到桑叶多糖水溶液，再用乙醇溶液洗脱树脂柱得桑叶黄酮乙醇溶液，所得桑叶多糖水溶液采用活性炭脱色后醇沉干燥，可得桑叶多糖粉末，桑叶黄酮乙醇溶液干燥可得桑叶黄酮粉末，将桑叶生物碱溶液浓缩至浸膏后加入盐酸溶液充分提取，过滤后所得滤液用氨水调pH至范围为9～11，氯仿萃取，减压蒸馏去除氯仿，干燥后用正己烷洗涤可得桑叶生物碱粉末。c. Separation: After the obtained mulberry leaf water extract is adsorbed by a macroporous adsorption resin column, the resin column is first eluted with distilled water until it is colorless to obtain an aqueous solution of mulberry leaf polysaccharide, and then the resin column is eluted with ethanol solution to obtain mulberry leaf flavonoids Ethanol solution, the obtained mulberry leaf polysaccharide aqueous solution is decolorized with activated carbon and then alcohol-precipitated and dried to obtain mulberry leaf polysaccharide powder, and the mulberry leaf flavonoids ethanol solution is dried to obtain mulberry leaf flavonoid powder, and the mulberry leaf alkaloid solution is concentrated to an extract, and then hydrochloric acid solution is added Fully extract, filter and adjust the pH of the obtained filtrate to a range of 9-11 with ammonia water, extract with chloroform, distill under reduced pressure to remove chloroform, wash with n-hexane after drying to obtain mulberry leaf alkaloid powder.
上所述桑叶为白桑、鲁桑或鸡桑。The above-mentioned mulberry leaves are white mulberry, lusang or chicken mulberry.
上述水浸提桑叶粉过程中：浸提温度为60～90℃，水的pH范围为7～10，桑叶粉与水的固液比范围为1:10～1:50。In the process of extracting mulberry leaf powder by water leaching: the extraction temperature is 60-90° C., the pH range of water is 7-10, and the solid-to-liquid ratio of mulberry leaf powder to water is in the range of 1:10-1:50.
上述盐酸-乙醇-水溶液提取桑叶残渣过程中：盐酸-乙醇-水溶液中盐酸的体积分数范围为1％～3％、乙醇的体积分数范围为40％～80％，桑叶残渣与盐酸-乙醇-水溶液的固液比范围为1:10～1:50。In the above-mentioned hydrochloric acid-ethanol-water solution extraction mulberry leaf residue process: the volume fraction scope of hydrochloric acid in the hydrochloric acid-ethanol-water solution is 1%～3%, the volume fraction scope of ethanol is 40%～80%, mulberry leaf residue and hydrochloric acid-ethanol - The solid-to-liquid ratio of the aqueous solution ranges from 1:10 to 1:50.
上述桑叶水提液的总黄酮的含量范围为2～8mg/mL、总多糖的含量范围为2.5～10mg/mL。The content range of the total flavonoids in the above mulberry leaf water extract is 2-8 mg/mL, and the content range of the total polysaccharides is 2.5-10 mg/mL.
上述盐酸溶液提取过程中：盐酸的体积浓度范围为0.3％～1％。During the above hydrochloric acid solution extraction process: the volume concentration range of hydrochloric acid is 0.3%-1%.
上述大孔吸附树脂为交联聚苯乙烯大孔吸附树脂或交联聚丙烯酸酯大孔吸附树脂。The above-mentioned macroporous adsorption resin is a cross-linked polystyrene macroporous adsorption resin or a cross-linked polyacrylate macroporous adsorption resin.
上述洗脱桑叶黄酮所用的乙醇溶液的体积浓度范围为50％～70％。The volume concentration range of the ethanol solution used for eluting the mulberry leaf flavonoids is 50%-70%.
上述氯仿萃取次数范围为1～10。The above-mentioned chloroform extraction number ranges from 1 to 10.
上述正己烷洗涤次数范围为1～3。The above-mentioned n-hexane washing times range from 1 to 3.
有益效果：Beneficial effect:
(1)本发明采用联产所得桑叶黄酮、桑叶多糖和桑叶生物碱的复合提取方法条件温和，能耗低污染小，所用的大孔吸附树脂和氯仿经再生可重复使用，所得的有效组分经济价值极高，大大的节约了桑叶资源，开辟了桑叶这类农副产品的利用的新途径，提高了桑叶资源的药用利用率和经济附加值。(1) The present invention adopts the compound extraction method condition of co-production gained mulberry leaf flavonoids, mulberry leaf polysaccharide and mulberry leaf alkaloid, low energy consumption and little pollution, used macroporous adsorption resin and chloroform can be reused through regeneration, and the obtained The effective components have extremely high economic value, greatly save mulberry leaf resources, open up a new way to utilize agricultural and sideline products such as mulberry leaves, and improve the medicinal utilization rate and economic added value of mulberry leaf resources.
(2)本发明采用的复合提取工艺采用碱水提法提取桑叶黄酮和多糖，可在同时获得桑叶黄酮和多糖的基础上进一步分离桑叶生物碱，且所用的提取液为弱碱溶液，对桑叶黄酮和多糖理化性质无影响，而碱水溶液破坏了植物细胞的纤维组织，利于后期桑叶生物碱的提取。(2) The composite extraction process that the present invention adopts adopts alkaline water extraction to extract mulberry leaf flavonoids and polysaccharides, and can further separate mulberry leaf alkaloids on the basis of simultaneously obtaining mulberry leaf flavonoids and polysaccharides, and the extract used is a weak alkali solution , has no effect on the physical and chemical properties of mulberry leaf flavonoids and polysaccharides, but the alkaline aqueous solution destroys the fibrous tissue of plant cells, which is beneficial to the extraction of mulberry leaf alkaloids in the later stage.
(3)本发明采用树脂吸附法分离桑叶黄酮和多糖，可同时除去大量杂质，并有效的分离两种有效组分，树脂吸附分离法操作简单，易于工业生产放大。(3) The present invention adopts the resin adsorption method to separate the mulberry leaf flavonoids and polysaccharides, which can simultaneously remove a large amount of impurities and effectively separate the two effective components. The resin adsorption separation method is simple to operate and easy to scale up in industrial production.
(4)本发明采用的以提取桑叶黄酮和多糖后的桑叶残渣为原料，经再次提取获得桑叶生物碱的方法可有效的获得桑叶生物碱，且所得生物碱溶液中杂质含量较少，浓缩后的浸膏经盐酸再次提取后可大大提高桑叶生物碱的纯度。(4) The mulberry leaf residue that the present invention adopts after extracting mulberry leaf flavonoids and polysaccharides is raw material, and the method for obtaining mulberry leaf alkaloids through extraction again can effectively obtain mulberry leaf alkaloids, and the impurity content is relatively high in the gained alkaloid solution Less, the concentrated extract can greatly improve the purity of mulberry leaf alkaloids after being extracted again with hydrochloric acid.
(5)本发明采用的氯仿萃取桑叶生物碱的方法可同时完成除杂和富集两部分操作，且氯仿对桑叶总生物碱的选择性较大，经多次萃取可完全萃得桑叶中含量较低但经济价值极高的DNJ等桑叶生物碱有效组分，使桑叶的经济价值显著提高。(5) The method for extracting mulberry leaf alkaloids with chloroform used in the present invention can simultaneously complete the two-part operation of impurity removal and enrichment, and the selectivity of chloroform to the total alkaloids of mulberry leaves is relatively large, and mulberry leaves can be completely extracted through multiple extractions. The effective components of mulberry leaf alkaloids such as DNJ with low content in leaves but high economic value can significantly increase the economic value of mulberry leaves.
四、附图说明 4. Description of drawings
图1联产桑叶黄酮、多糖及生物碱的复合提取工艺流程图Fig. 1 co-production process flow chart of compound extraction of mulberry leaf flavonoids, polysaccharides and alkaloids
五、具体实施方式 5. Specific implementation
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。Below in conjunction with specific embodiment, further illustrate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.
实施例1Example 1
选用白桑桑叶为原料，经洗净晒干后60℃下烘干至变脆，粉碎后过筛(筛径40～80目)获得桑叶粉。将桑叶粉在温度60℃、固液比1:10、pH7的条件用水浸提后过滤获得桑叶水提液和桑叶残渣，将桑叶残渣按固液比1:10加入盐酸-乙醇-水溶液(含盐酸1％、乙醇40％，体积分数)，提取获得含桑叶生物碱的溶液，所得桑叶水提液中桑叶黄酮含量为2.5mg/mL，桑叶多糖含量为2.0mg/mL。将所得桑叶水提液通过交联聚苯乙烯大孔吸附树脂柱进行吸附后，先用蒸馏水洗脱树脂柱至无色，得到桑叶多糖水溶液，再用50％(体积分数)乙醇溶液洗脱树脂柱得桑叶黄酮乙醇溶液。所得桑叶多糖水溶液采用活性炭脱色后醇沉干燥，可得桑叶多糖粉末，桑叶黄酮乙醇溶液干燥可得桑叶黄酮粉末。将桑叶生物碱溶液浓缩至浸膏后加入0.3％(体积分数)盐酸溶液充分提取，过滤后所得滤液用氨水调pH至9，氯仿萃取1次，减压蒸馏去除氯仿，干燥后用正己烷洗涤1次可得桑叶生物碱粉末。其中，桑叶黄酮检测方法：以芦丁为对照品，采用三氯化铝显色法分光光度计在510nm测定；桑叶多糖检测方法：以葡萄糖为对照品，采用硫酸苯酚法分光光度计在490nm测定；桑叶生物碱检测方法：以1-脱氧野尻霉素(1-DNJ)为对照品，采用溴甲酚绿染色法分光光度计在415nm测定。所得桑叶黄酮纯度为75.21％，桑叶多糖纯度为44.36％，桑叶生物碱纯度为32.98％。White mulberry leaves are selected as raw materials, washed and dried at 60°C until they become brittle, crushed and sieved (with a sieve diameter of 40-80 mesh) to obtain mulberry leaf powder. Extract the mulberry leaf powder with water at a temperature of 60°C, a solid-to-liquid ratio of 1:10, and a pH of 7, then filter to obtain the mulberry leaf water extract and mulberry leaf residue, and add the mulberry leaf residue to hydrochloric acid-ethanol at a solid-to-liquid ratio of 1:10 -Aqueous solution (containing 1% hydrochloric acid, 40% ethanol, volume fraction), extracting to obtain a solution containing mulberry leaf alkaloids, the content of mulberry leaf flavonoids in the obtained mulberry leaf water extract is 2.5mg/mL, and the content of mulberry leaf polysaccharides is 2.0mg /mL. After the obtained mulberry leaf water extract is adsorbed by a cross-linked polystyrene macroporous adsorption resin column, the resin column is first eluted to colorless with distilled water to obtain an aqueous solution of mulberry leaf polysaccharide, and then washed with 50% (volume fraction) ethanol solution The ethanol solution of mulberry leaf flavonoids was obtained by deresinizing the column. The obtained mulberry leaf polysaccharide aqueous solution is decolorized by activated carbon, and then alcohol-precipitated and dried to obtain mulberry leaf polysaccharide powder, and the mulberry leaf flavonoid ethanol solution is dried to obtain mulberry leaf flavonoid powder. Concentrate the mulberry leaf alkaloid solution to the extract, add 0.3% (volume fraction) hydrochloric acid solution to fully extract, filter the obtained filtrate to adjust the pH to 9 with ammonia water, extract once with chloroform, distill under reduced pressure to remove chloroform, dry it with n-hexane Wash once to get mulberry leaf alkaloid powder. Among them, the detection method of mulberry leaf flavonoids: taking rutin as the reference substance, adopting the aluminum chloride chromogenic method spectrophotometer to measure at 510nm; the detection method of mulberry leaf polysaccharide: using glucose as the reference substance, using the sulfuric acid phenol method spectrophotometer Determination at 490nm; detection method of mulberry leaf alkaloids: with 1-deoxynojirimycin (1-DNJ) as the reference substance, bromocresol green staining spectrophotometer was used to measure at 415nm. The obtained mulberry leaf flavones have a purity of 75.21%, the mulberry leaf polysaccharides have a purity of 44.36%, and the mulberry leaf alkaloids have a purity of 32.98%.
实施例2Example 2
选用鲁桑桑叶为原料，经洗净晒干后60℃下烘干至变脆，粉碎后过筛(筛径40～80目)获得桑叶粉。将桑叶粉在温度90℃、固液比1:50、pH10的条件用水浸提后过滤获得桑叶水提液和桑叶残渣，将桑叶残渣按固液比1:50加入盐酸-乙醇-水溶液(含盐酸3％、乙醇80％，体积分数)，提取获得含桑叶生物碱的溶液，所得桑叶水提液中桑叶黄酮含量为3.2mg/mL，桑叶多糖含量为2.8mg/mL。将所得桑叶水提液通过交联聚苯乙烯大孔吸附树脂柱进行吸附后，先用蒸馏水洗脱树脂柱至无色，得到桑叶多糖水溶液，再用70％(体积分数)乙醇溶液洗脱树脂柱得桑叶黄酮乙醇溶液。所得桑叶多糖水溶液采用活性炭脱色后醇沉干燥，可得桑叶多糖粉末，桑叶黄酮乙醇溶液干燥可得桑叶黄酮粉末。将桑叶生物碱溶液浓缩至浸膏后加入1％(体积分数)盐酸溶液充分提取，过滤后所得滤液用氨水调pH至11，氯仿萃取10次，减压蒸馏去除氯仿，干燥后用正己烷洗涤3次可得桑叶生物碱粉末。所得桑叶黄酮纯度为73.37％，桑叶多糖纯度为48.11％，桑叶生物碱纯度为38.48％。The mulberry leaf is selected as raw material, washed and dried at 60°C until it becomes brittle, crushed and sieved (with a sieve diameter of 40-80 mesh) to obtain the mulberry leaf powder. Extract the mulberry leaf powder with water at a temperature of 90°C, a solid-to-liquid ratio of 1:50, and a pH of 10, and then filter to obtain the mulberry leaf water extract and mulberry leaf residue. Add the mulberry leaf residue to hydrochloric acid-ethanol at a solid-to-liquid ratio of 1:50 -Aqueous solution (containing 3% hydrochloric acid, 80% ethanol, volume fraction), extracting to obtain a solution containing mulberry leaf alkaloids, the content of mulberry leaf flavonoids in the obtained mulberry leaf water extract is 3.2mg/mL, and the content of mulberry leaf polysaccharides is 2.8mg /mL. After the obtained mulberry leaf water extract is adsorbed by a cross-linked polystyrene macroporous adsorption resin column, the resin column is first eluted to colorless with distilled water to obtain an aqueous solution of mulberry leaf polysaccharide, and then washed with 70% (volume fraction) ethanol solution The ethanol solution of mulberry leaf flavonoids was obtained by deresinizing the column. The obtained mulberry leaf polysaccharide aqueous solution is decolorized by activated carbon, and then alcohol-precipitated and dried to obtain mulberry leaf polysaccharide powder, and the mulberry leaf flavonoid ethanol solution is dried to obtain mulberry leaf flavonoid powder. Concentrate the mulberry leaf alkaloid solution to the extract, add 1% (volume fraction) hydrochloric acid solution to fully extract, filter the obtained filtrate to adjust the pH to 11 with ammonia water, extract 10 times with chloroform, distill under reduced pressure to remove chloroform, dry it with n-hexane Wash 3 times to get mulberry leaf alkaloid powder. The obtained mulberry leaf flavones have a purity of 73.37%, the mulberry leaf polysaccharides have a purity of 48.11%, and the mulberry leaf alkaloids have a purity of 38.48%.
实施例3Example 3
选用鸡桑桑叶为原料，经洗净晒干后60℃下烘干至变脆，粉碎后过筛(筛径40～80目)获得桑叶粉。将桑叶粉在温度85℃、固液比1:40、pH8的条件用水浸提后过滤获得桑叶水提液和桑叶残渣，将桑叶残渣按固液比1:30加入盐酸-乙醇-水溶液(含盐酸1.5％、乙醇65％，体积分数)，提取获得含桑叶总生物碱的溶液，所得桑叶水提液中桑叶总黄酮含量为2.8mg/mL，桑叶总多糖含量为2.9mg/mL。将所得桑叶水提液通过交联聚丙烯酸酯大孔吸附树脂柱进行吸附后，先用蒸馏水洗脱树脂柱至无色，得到桑叶多糖水溶液，再用65％(体积分数)乙醇溶液洗脱树脂柱得桑叶黄酮乙醇溶液。所得桑叶多糖水溶液采用活性炭脱色后醇沉干燥，可得桑叶多糖粉末，桑叶黄酮乙醇溶液干燥可得桑叶黄酮粉末。将桑叶生物碱溶液浓缩至浸膏后加入0.8％(体积分数)盐酸溶液充分提取，过滤后所得滤液用氨水调pH至9，氯仿萃取8次，减压蒸馏去除氯仿，干燥后用正己烷洗涤2次可得桑叶生物碱粉末。所得桑叶黄酮纯度为76.22％，桑叶多糖纯度为44.41％，桑叶生物碱纯度为31.02％。The mulberry leaf is selected as the raw material, washed and dried at 60° C. until it becomes brittle, crushed and sieved (with a sieve diameter of 40 to 80 mesh) to obtain the mulberry leaf powder. Extract the mulberry leaf powder with water at a temperature of 85°C, a solid-to-liquid ratio of 1:40, and a pH of 8, and then filter to obtain the mulberry leaf water extract and mulberry leaf residue. Add the mulberry leaf residue to hydrochloric acid-ethanol at a solid-to-liquid ratio of 1:30 -Aqueous solution (containing hydrochloric acid 1.5%, ethanol 65%, volume fraction), extraction obtains the solution containing the total alkaloids of mulberry leaves, the total flavonoid content of mulberry leaves in the obtained mulberry leaf water extract is 2.8mg/mL, and the total polysaccharide content of mulberry leaves It was 2.9 mg/mL. After the obtained mulberry leaf water extract is adsorbed by a cross-linked polyacrylate macroporous adsorption resin column, the resin column is first eluted to colorless with distilled water to obtain an aqueous solution of mulberry leaf polysaccharide, and then washed with 65% (volume fraction) ethanol solution The ethanol solution of mulberry leaf flavonoids was obtained by deresinizing the column. The obtained mulberry leaf polysaccharide aqueous solution is decolorized by activated carbon, and then alcohol-precipitated and dried to obtain mulberry leaf polysaccharide powder, and the mulberry leaf flavonoid ethanol solution is dried to obtain mulberry leaf flavonoid powder. Concentrate the mulberry leaf alkaloid solution to the extract, add 0.8% (volume fraction) hydrochloric acid solution to fully extract, filter the obtained filtrate to adjust the pH to 9 with ammonia water, extract 8 times with chloroform, distill under reduced pressure to remove chloroform, dry it with n-hexane Wash twice to get mulberry leaf alkaloid powder. The obtained mulberry leaf flavones have a purity of 76.22%, the mulberry leaf polysaccharides have a purity of 44.41%, and the mulberry leaf alkaloids have a purity of 31.02%.
实施例4Example 4
选用白桑桑叶为原料，经洗净晒干后60℃下烘干至变脆，粉碎后过筛(筛径40～80目)获得桑叶粉。将桑叶粉在温度70℃、固液比1:30、pH9的条件用水浸提后过滤获得桑叶水提液和桑叶残渣，将桑叶残渣按固液比1:40加入盐酸-乙醇-水溶液(含盐酸2％、乙醇75％，体积分数)，提取获得含桑叶生物碱的溶液，所得桑叶水提液中桑叶黄酮含量为5.7mg/mL，桑叶多糖含量为4.2mg/mL。将所得桑叶水提液通过交联聚丙烯酸酯大孔吸附树脂柱进行吸附后，先用蒸馏水洗脱树脂柱至无色，得到桑叶多糖水溶液，再用55％(体积分数)乙醇溶液洗脱树脂柱得桑叶黄酮乙醇溶液。所得桑叶多糖水溶液采用活性炭脱色后醇沉干燥，可得桑叶多糖粉末，桑叶黄酮乙醇溶液干燥可得桑叶黄酮粉末。将桑叶生物碱溶液浓缩至浸膏后加入0.5％(体积分数)盐酸溶液充分提取，过滤后所得滤液用氨水调pH至10，氯仿萃取6次，减压蒸馏去除氯仿，干燥后用正己烷洗涤1次可得桑叶生物碱粉末。所得桑叶黄酮纯度为74.22％，桑叶多糖纯度为56.91％，桑叶生物碱纯度为45.65％。White mulberry leaves are selected as raw materials, washed and dried at 60°C until they become brittle, crushed and sieved (with a sieve diameter of 40-80 mesh) to obtain mulberry leaf powder. Extract the mulberry leaf powder with water at a temperature of 70°C, a solid-to-liquid ratio of 1:30, and a pH of 9, and then filter to obtain the mulberry leaf water extract and mulberry leaf residue. Add the mulberry leaf residue to hydrochloric acid-ethanol at a solid-to-liquid ratio of 1:40 -Aqueous solution (containing 2% hydrochloric acid, 75% ethanol, volume fraction), extracting to obtain a solution containing mulberry leaf alkaloids, the content of mulberry leaf flavonoids in the obtained mulberry leaf water extract is 5.7mg/mL, and the content of mulberry leaf polysaccharides is 4.2mg /mL. After the obtained mulberry leaf water extract is adsorbed by a cross-linked polyacrylate macroporous adsorption resin column, the resin column is first eluted to colorless with distilled water to obtain an aqueous solution of mulberry leaf polysaccharide, and then washed with 55% (volume fraction) ethanol solution The ethanol solution of mulberry leaf flavonoids was obtained by deresinizing the column. The obtained mulberry leaf polysaccharide aqueous solution is decolorized by activated carbon, and then alcohol-precipitated and dried to obtain mulberry leaf polysaccharide powder, and the mulberry leaf flavonoid ethanol solution is dried to obtain mulberry leaf flavonoid powder. Concentrate the mulberry leaf alkaloid solution to the extract, add 0.5% (volume fraction) hydrochloric acid solution to fully extract, filter the obtained filtrate to adjust the pH to 10 with ammonia water, extract 6 times with chloroform, distill under reduced pressure to remove chloroform, dry it with n-hexane Wash once to get mulberry leaf alkaloid powder. The obtained mulberry leaf flavones have a purity of 74.22%, the mulberry leaf polysaccharides have a purity of 56.91%, and the mulberry leaf alkaloids have a purity of 45.65%.
实施例5Example 5
选用白桑桑叶为原料，经洗净晒干后60℃下烘干至变脆，粉碎后过筛(筛径40～80目)获得桑叶粉。将桑叶粉在温度80℃、固液比1:20、pH10的条件用水浸提后过滤获得桑叶水提液和桑叶残渣，将桑叶残渣按固液比1:30加入盐酸-乙醇-水溶液(含盐酸2.5％、乙醇70％，体积分数)，提取获得含桑叶生物碱的溶液，所得桑叶水提液中桑叶黄酮含量为6.1mg/mL，桑叶多糖含量为5.9mg/mL。将所得桑叶水提液通过交联聚苯乙烯大孔吸附树脂柱进行吸附后，先用蒸馏水洗脱树脂柱至无色，得到桑叶多糖水溶液，再用50％(体积分数)乙醇溶液洗脱树脂柱得桑叶黄酮乙醇溶液。所得桑叶多糖水溶液采用活性炭脱色后醇沉干燥，可得桑叶多糖粉末，桑叶黄酮乙醇溶液干燥可得桑叶黄酮粉末。将桑叶生物碱溶液浓缩至浸膏后加入0.7％(体积分数)盐酸溶液充分提取，过滤后所得滤液用氨水调pH至9.5，氯仿萃取9次，减压蒸馏去除氯仿，干燥后用正己烷洗涤3次可得桑叶生物碱粉末。所得桑叶黄酮纯度为76.52％，桑叶多糖纯度为58.74％，桑叶生物碱纯度为47.63％。White mulberry leaves are selected as raw materials, washed and dried at 60°C until they become brittle, crushed and sieved (with a sieve diameter of 40-80 mesh) to obtain mulberry leaf powder. Extract the mulberry leaf powder with water at a temperature of 80°C, a solid-to-liquid ratio of 1:20, and a pH of 10, and then filter to obtain the mulberry leaf water extract and mulberry leaf residue. Add the mulberry leaf residue to hydrochloric acid-ethanol at a solid-to-liquid ratio of 1:30 -Aqueous solution (containing 2.5% hydrochloric acid, 70% ethanol, volume fraction), extracting to obtain a solution containing mulberry leaf alkaloids, the content of mulberry leaf flavonoids in the obtained mulberry leaf water extract is 6.1mg/mL, and the content of mulberry leaf polysaccharides is 5.9mg /mL. After the obtained mulberry leaf water extract is adsorbed by a cross-linked polystyrene macroporous adsorption resin column, the resin column is first eluted to colorless with distilled water to obtain an aqueous solution of mulberry leaf polysaccharide, and then washed with 50% (volume fraction) ethanol solution The ethanol solution of mulberry leaf flavonoids was obtained by deresinizing the column. The obtained mulberry leaf polysaccharide aqueous solution is decolorized by activated carbon, and then alcohol-precipitated and dried to obtain mulberry leaf polysaccharide powder, and the mulberry leaf flavonoid ethanol solution is dried to obtain mulberry leaf flavonoid powder. Concentrate the mulberry leaf alkaloid solution to the extract, add 0.7% (volume fraction) hydrochloric acid solution to fully extract, filter the obtained filtrate to adjust the pH to 9.5 with ammonia water, extract 9 times with chloroform, distill under reduced pressure to remove chloroform, dry it with n-hexane Wash 3 times to get mulberry leaf alkaloid powder. The obtained mulberry leaf flavones have a purity of 76.52%, the mulberry leaf polysaccharides have a purity of 58.74%, and the mulberry leaf alkaloids have a purity of 47.63%.
实施例6Example 6
选用白桑桑叶为原料，经洗净晒干后60℃下烘干至变脆，粉碎后过筛(筛径40～80目)获得桑叶粉。将桑叶粉在温度65℃、固液比1:40、pH8的条件用水浸提后过滤获得桑叶水提液和桑叶残渣，将桑叶残渣按固液比1:30加入盐酸-乙醇-水溶液(含盐酸2％、乙醇70％，体积分数)，提取获得含桑叶生物碱的溶液，所得桑叶水提液中桑叶黄酮含量为5.6mg/mL，桑叶多糖含量为4.8mg/mL。将所得桑叶水提液通过交联聚丙烯酸酯大孔吸附树脂柱进行吸附后，先用蒸馏水洗脱树脂柱至无色，得到桑叶多糖水溶液，再用60％(体积分数)乙醇溶液洗脱树脂柱得桑叶黄酮乙醇溶液。所得桑叶多糖水溶液采用活性炭脱色后醇沉干燥，可得桑叶多糖粉末，桑叶黄酮乙醇溶液干燥可得桑叶黄酮粉末。将桑叶生物碱溶液浓缩至浸膏后加入0.9％(体积分数)盐酸溶液充分提取，过滤后所得滤液用氨水调pH至10，氯仿萃取6次，减压蒸馏去除氯仿，干燥后用正己烷洗涤3次可得桑叶生物碱粉末。所得桑叶黄酮纯度为77.79％，桑叶多糖纯度为54.23％，桑叶生物碱纯度为42.46％。White mulberry leaves are selected as raw materials, washed and dried at 60°C until they become brittle, crushed and sieved (with a sieve diameter of 40-80 mesh) to obtain mulberry leaf powder. Extract the mulberry leaf powder with water at a temperature of 65°C, a solid-to-liquid ratio of 1:40, and a pH of 8, then filter to obtain the mulberry leaf water extract and mulberry leaf residue, and add the mulberry leaf residue to hydrochloric acid-ethanol at a solid-to-liquid ratio of 1:30 -Aqueous solution (containing 2% hydrochloric acid, 70% ethanol, volume fraction), extracting to obtain a solution containing mulberry leaf alkaloids, the content of mulberry leaf flavonoids in the obtained mulberry leaf water extract is 5.6mg/mL, and the content of mulberry leaf polysaccharides is 4.8mg /mL. After the obtained mulberry leaf water extract is adsorbed by a cross-linked polyacrylate macroporous adsorption resin column, the resin column is first eluted to colorless with distilled water to obtain an aqueous solution of mulberry leaf polysaccharide, and then washed with 60% (volume fraction) ethanol solution The ethanol solution of mulberry leaf flavonoids was obtained by deresinizing the column. The obtained mulberry leaf polysaccharide aqueous solution is decolorized by activated carbon, and then alcohol-precipitated and dried to obtain mulberry leaf polysaccharide powder, and the mulberry leaf flavonoid ethanol solution is dried to obtain mulberry leaf flavonoid powder. Concentrate the mulberry leaf alkaloid solution to extract, add 0.9% (volume fraction) hydrochloric acid solution to fully extract, filter the obtained filtrate to adjust the pH to 10 with ammonia water, extract 6 times with chloroform, distill under reduced pressure to remove chloroform, dry it with n-hexane Wash 3 times to get mulberry leaf alkaloid powder. The obtained mulberry leaf flavones have a purity of 77.79%, the mulberry leaf polysaccharides have a purity of 54.23%, and the mulberry leaf alkaloids have a purity of 42.46%.
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