CN1066055C - Production method for extracting flavonoid compound extract or powder from bamboo leaf - Google Patents
Production method for extracting flavonoid compound extract or powder from bamboo leaf Download PDFInfo
- Publication number
- CN1066055C CN1066055C CN98104564A CN98104564A CN1066055C CN 1066055 C CN1066055 C CN 1066055C CN 98104564 A CN98104564 A CN 98104564A CN 98104564 A CN98104564 A CN 98104564A CN 1066055 C CN1066055 C CN 1066055C
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- Prior art keywords
- bamboo
- extract
- extraction
- powder
- flavonoid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
本发明属于一种从植物中提取黄酮类化合物,尤其是从竹叶中提取黄酮类化合物浸膏或粉剂的生产方法。以竹叶为原料,通过提取、浓缩、分离、精制、或再干燥所得的产品,含有大量的竹叶黄酮糖苷,及植物酚酸、蒽醌类、萜类内酯等化合物。该制剂具有优良的抗自由基、抗氧化、抗衰老和降血脂等作用,并带有典型的竹子芳香,可广泛地应用于各种老年功能性食品和医药保健品。该制剂是用低浓度的低级醇为溶剂热回流提取,用中级醇液~液萃取进行精制。生产过程安全、简便,无污染,易于控制,适于大规模的工业化生产,同时还具有黄酮提取率高、纯度好等特点。The invention belongs to a production method for extracting flavonoid compounds from plants, in particular extracting flavonoid compound extract or powder from bamboo leaves. Using bamboo leaves as raw materials, the products obtained through extraction, concentration, separation, refining, or re-drying contain a large amount of bamboo leaf flavonoid glycosides, and compounds such as plant phenolic acids, anthraquinones, and terpene lactones. The preparation has excellent anti-free radical, anti-oxidation, anti-aging and hypolipidemic effects, and has a typical bamboo aroma, and can be widely used in various functional foods for the elderly and medical and health products. The preparation is extracted by heat reflux with low-concentration lower alcohol as solvent, and refined by liquid-liquid extraction with middle alcohol. The production process is safe, simple, pollution-free, easy to control, suitable for large-scale industrial production, and also has the characteristics of high flavonoid extraction rate and good purity.
Description
本发明涉及一种从植物中提取黄酮类化合物的生产方法,尤其是从从竹叶中提取黄酮类化合物浸膏或粉剂的生产方法。The invention relates to a production method for extracting flavonoids from plants, in particular to a production method for extracting flavonoids extract or powder from bamboo leaves.
生物黄酮广泛存在于植物界,是许多中草药的有效成分。除了从银杏叶、法国松树皮、日本杜仲中提取黄酮类制剂以外,葛根、甘草、山楂、茶叶、柿叶、马尾松针及松实、桂皮、合欢皮、枸杞根皮茎叶、石斛、虫草、首乌、桔皮、五味子、枣、花生壳、稻根、茄杆等内含的生物黄酮均具有开发价值。以当今生产和使用规模最大的银杏黄酮为例,其生产工艺大致为以下3种类型:Bioflavonoids widely exist in the plant kingdom and are the active ingredients of many Chinese herbal medicines. In addition to extracting flavonoids from ginkgo leaves, French pine bark, and Japanese eucommia, kudzu root, licorice, hawthorn, tea, persimmon leaves, masson pine needles and pine nuts, cinnamon bark, acacia bark, wolfberry root bark stems and leaves, dendrobium, cordyceps, The bioflavonoids contained in Shouwu, orange peel, Schisandra chinensis, dates, peanut shells, rice roots, eggplant stems, etc. all have development value. Taking ginkgo flavonoids, which is produced and used on the largest scale today, as an example, its production process roughly falls into the following three types:
(1)水蒸汽蒸馏法:将银杏叶干燥、粉碎后,100~120℃水蒸汽蒸馏,蒸馏液冷却后,用非极性大孔树脂(或其他吸附剂)吸附,然后用乙醇洗脱,蒸干即得粉状结晶。该方法设备简单,但提取率低,现已很少采用。(1) Steam distillation method: after drying and pulverizing Ginkgo biloba leaves, steam distillation at 100-120°C, after the distillate is cooled, adsorb with non-polar macroporous resin (or other adsorbents), and then elute with ethanol, Evaporate to dryness to obtain powdery crystals. This method has simple equipment, but the extraction rate is low, so it is rarely used now.
(2)有机溶剂萃取:这是目前国内外使用最广泛的方法,其提取工艺的专利也较多[从银杏叶中提取黄酮类化合物的方法,李兆龙,中草药,1992,14(6):5-6],可归纳为两种形式。一种是制备粗提物:把银杏叶干燥、粉碎后用有机溶剂(如乙醇或丙酮)提取,过滤、减压浓缩回收溶剂后,即得银杏浸膏。这种方法生产设备简单,产品得率高(约12~14%),但含大量的杂质,通常呈棕黑色,制品的总黄酮含量为7~10%。另一种是制备精提物:这类方法通常在粗提物的基础上进一步精制,常用的精制方法有:液~液萃取(例如用二氯甲烷、氯仿、石油醚或苯脱脂;或用丁酮、丙酮-丁酮或乙酸乙酯萃取),沉淀法(用氨水或氢氧化铅沉淀)和吸附~解析法(用大孔树脂、硅藻土或硅胶等吸附剂吸附,乙醇洗脱)。再通过无水硫酸钠干燥、过滤、减压蒸馏除去溶剂后,即可得精提物。一般为黄褐色粉末,得率约1~3%,总黄酮含量约为20~26%。(2) Organic solvent extraction: this is the most widely used method at home and abroad, and there are many patents on its extraction process [method for extracting flavonoids from ginkgo leaves, Li Zhaolong, Chinese herbal medicine, 1992, 14 (6): 5 -6], which can be summarized into two forms. One is to prepare the crude extract: dry and pulverize the ginkgo leaves, extract with an organic solvent (such as ethanol or acetone), filter, concentrate under reduced pressure and recover the solvent to obtain the ginkgo extract. This method has simple production equipment and high product yield (about 12-14%), but contains a large amount of impurities, usually brownish black, and the total flavonoid content of the product is 7-10%. The other is to prepare the fine extract: this type of method is usually further refined on the basis of the crude extract, and the commonly used refining methods are: liquid-liquid extraction (such as degreasing with dichloromethane, chloroform, petroleum ether or benzene; or using Butanone, acetone-butanone or ethyl acetate extraction), precipitation method (precipitation with ammonia water or lead hydroxide) and adsorption-analysis method (adsorption with adsorbents such as macroporous resin, diatomaceous earth or silica gel, ethanol elution) . After drying with anhydrous sodium sulfate, filtering, and distilling off the solvent under reduced pressure, the fine extract can be obtained. It is generally yellowish-brown powder, the yield is about 1-3%, and the total flavonoid content is about 20-26%.
(3)超临界流体萃取:近10年来,用该技术提取天然植物中的药用有效成分越来越受到关注,它和上述工艺相比,具有提取效率高、无溶剂残留、活性成分不易被分解和破坏等优点。欧洲专利EP0308675(1988)报道了用超临界CO2提取银杏叶中有效成分的方法,国内近年来也在这方面做了不少工作,但大多处在实验室研究阶段,未见有工业化应用的报道。(3) Supercritical fluid extraction: In the past 10 years, more and more attention has been paid to using this technology to extract medicinal active ingredients in natural plants. Compared with the above-mentioned processes, it has high extraction efficiency, no solvent residue, and the active ingredients are not easily extracted Advantages such as decomposition and destruction. European patent EP0308675 (1988) reported a method for extracting active ingredients in ginkgo leaves with supercritical CO2. A lot of work has been done in this area in China in recent years, but most of them are in the stage of laboratory research, and there are no reports of industrial applications. .
竹子是禾本科(Poaceae)竹亚科(Bambusoideae)多年生常绿植物,是一种大众化的药、食两用植物。竹子在东南亚广为分布,我国是世界竹子的中心产区之一,现有竹种300多种,竹林面积6000多万亩。竹子的医疗保健作用早已为我国劳动人民所认识,《本草求真》曰:“竹叶据书载,凉心缓脾、清痰止渴,为治上焦风邪烦热、咳逆喘促、呕哕吐血、一切中风惊痫等症,无非因其轻能解上、辛能散郁、甘能缓脾、凉能入心、寒能疗热故耳”。淡竹叶和淡竹沥就是中医一味传统的清热解毒药。竹子全身是宝,是当今世界最具有使用价值的植物之一。但在竹子的综合利用中,竹叶的研究和开发明显滞后,除极少量的药用和食用以外,基本上处于原始状态。近年来,发明人对竹叶的有效成分及其生物活性进行了系统的研究,发现竹叶中含有丰富的黄酮等酚性化合物、蒽醌类化合物、萜类内酯、免疫活性多糖、特种氨基酸(δ-羟基赖氨酸)和锰、锌、铁、硒等微量元素,其中黄酮类化合物是其主要的功能成分。竹叶所含的黄酮类化合物基本上皆是黄酮糖苷,相当部分是碳苷黄酮,如荭草苷木糖苷、异荭草苷、4’-甲氧基-牡荆苷等。Bamboo is a perennial evergreen plant of the Poaceae (Poaceae) bamboo subfamily (Bambusoideae), and is a popular medicine and food dual-purpose plant. Bamboo is widely distributed in Southeast Asia. my country is one of the central production areas of bamboo in the world. There are more than 300 kinds of bamboo species and more than 60 million mu of bamboo forest area. The medical and health care function of bamboo has long been recognized by the working people in our country. "Materia Medica Seeking Truth" says: "Bamboo leaves cool the heart and relieve the spleen, clear phlegm and quench thirst. , vomiting, vomiting blood, and all strokes and convulsions, etc., are nothing more than because lightness can relieve the upper body, pungentness can relieve depression, sweetness can relieve the spleen, coolness can enter the heart, and coldness can heal heat.” Danzhuye and Danzhuli are traditional Chinese medicine for clearing away heat and detoxifying. The whole body of bamboo is a treasure, and it is one of the most valuable plants in the world today. However, in the comprehensive utilization of bamboo, the research and development of bamboo leaves obviously lag behind, except for a very small amount of medicinal and edible, it is basically in the original state. In recent years, the inventors have conducted systematic research on the active ingredients of bamboo leaves and their biological activities, and found that bamboo leaves are rich in flavonoids and other phenolic compounds, anthraquinones, terpenoid lactones, immune active polysaccharides, special amino acids (δ-hydroxylysine) and trace elements such as manganese, zinc, iron, selenium, among which flavonoids are its main functional components. The flavonoids contained in bamboo leaves are basically flavone glycosides, and a considerable part of them are carbon glycoside flavonoids, such as orientin xyloside, isoorientin, 4'-methoxy-vitexin, etc.
研究表明,竹叶提取物(Ebl)具有优良的抗自由基、抗氧化和抗衰老活性。大量的研究表明,Ebl具有很强的清除活性氧自由基和阻断亚硝化反应的能力;能显著诱导老龄小鼠内源性抗氧化酶系(SOD和GSH-Px)的活力、抑制脂质过氧化和清除过氧化产物;能显著增强小鼠的抗疲劳和抗应激能力;Ebl能显著降低大鼠血甘油三酯和总胆固醇的浓度,增加HDL-胆固醇浓度、降低LDL-胆固醇浓度,抑制大鼠体重的增加。动物试验的结果表明,Ebl降低血脂与诱导内源性SOD活力的作用与银杏叶提取物(Egb)相同,抑制脂质过氧化和诱导GSH-Px活力的作用明显优于Egb。此外,尚未从竹叶中检出有害成分或抗营养因子。急性毒性试验表明,Ebl经口的LD50>10g/kg体重,可视为实际无毒;Ames试验表明,Ebl无致突变性。所以说,Ebl是一种安全高效的生物黄酮保健因子,可广泛应用于功能性食品和多种老年退行性疾病的防治。Studies have shown that bamboo leaf extract (Ebl) has excellent anti-free radical, anti-oxidation and anti-aging activities. A large number of studies have shown that Ebl has a strong ability to scavenge active oxygen free radicals and block nitrosation reactions; it can significantly induce the activity of endogenous antioxidant enzymes (SOD and GSH-Px) in aged mice, inhibit lipid Peroxidation and removal of peroxidation products; can significantly enhance the anti-fatigue and anti-stress ability of mice; Ebl can significantly reduce the concentration of rat blood triglyceride and total cholesterol, increase the concentration of HDL-cholesterol, reduce the concentration of LDL-cholesterol, Inhibition of weight gain in rats. The results of animal experiments showed that the effect of Ebl on reducing blood lipid and inducing endogenous SOD activity was the same as that of ginkgo biloba extract (Egb), and the effect on inhibiting lipid peroxidation and inducing GSH-Px activity was significantly better than that of Egb. In addition, no harmful components or anti-nutritional factors have been detected from bamboo leaves. Acute toxicity test shows that the oral LD 50 of Ebl > 10g/kg body weight can be regarded as practically non-toxic; Ames test shows that Ebl has no mutagenicity. Therefore, Ebl is a safe and efficient bioflavonoid health factor, which can be widely used in the prevention and treatment of functional foods and various senile degenerative diseases.
本发明的目的在于利用我国资源十分丰富、且尚未得到有效开发利用的竹叶,提供一种工艺简便、提取率高,过程易控制、无污染、适合于大规模工业化生产的从竹叶中提取黄酮类化合物浸膏或粉剂的生产方法。The purpose of the present invention is to utilize bamboo leaves which are very rich in resources in my country and have not yet been effectively developed and utilized, to provide a kind of extraction from bamboo leaves with simple process, high extraction rate, easy control of the process, no pollution, and suitable for large-scale industrial production. The production method of flavonoid compound extract or powder.
从竹叶中提取黄酮类化合物浸膏或粉剂的生产方法,其特征是:以竹叶为原料,将竹叶洗净、烘干、破碎,用较低浓度(20-40%,体积百分浓度)的低级醇(甲醇或乙醇)为溶剂,以1∶10-15的固液比(重量百分比)热回流提取1-2小时,提取液浓缩后物理去杂,再用中级醇(丁醇或戊醇)液-液萃取,萃取液减压浓缩回收溶剂后,加少量水转溶,成黄酮类化合物浸膏,或再经真空或喷雾干燥,即制得黄酮类化合物粉剂。The production method of extracting flavonoids extract or powder from bamboo leaves is characterized in that: bamboo leaves are used as raw materials, the bamboo leaves are washed, dried, and broken, and a lower concentration (20-40%, volume percent) is used Concentration) of lower alcohol (methanol or ethanol) as solvent, with 1: 10-15 solid-liquid ratio (weight percent) hot reflux extraction 1-2 hours, after the extract is concentrated, physically remove impurities, and then use intermediate alcohol (butanol or amyl alcohol) liquid-liquid extraction, the extract is concentrated under reduced pressure to recover the solvent, then add a small amount of water to dissolve it, and form a flavonoid compound extract, or vacuum or spray drying to obtain a flavonoid compound powder.
本发明是这样实现的:The present invention is achieved like this:
竹叶→洗净→烘干→破碎→乙醇~水溶液热回流提取→过滤→减压浓缩→静止絮凝→分离去杂→正丁醇分步萃取→减压浓缩回收溶剂→热水转溶→减压浓缩→(浸膏)→真空或喷雾干燥→竹叶黄酮粉剂Bamboo leaves→washing→drying→crushing→ethanol~water solution hot reflux extraction→filtering→decompression concentration→static flocculation→separation and impurity removal→n-butanol step-by-step extraction→decompression concentration recovery solvent→hot water transfer→reduction Compression concentration→(extract)→vacuum or spray drying→bamboo leaf flavonoid powder
该发明的技术要点是根据竹叶黄酮类化合物的组成特点和理化特性(良好的亲水性和热稳定性)、采用乙醇水溶液一次性热回流提取;根据杂质在一定条件下的絮凝和沉淀特性,用物理方法分离去杂;然后用正丁醇分步萃取,回收溶剂,经水转溶后得浸膏,再干燥即得粉剂。工艺简捷,易于控制;设备投入少,分离效果好,提取率高;无有机溶剂残留,成品质量好;整个过程不使用有毒、有害试剂和强酸强碱,基本上无“三废”排放,不构成环境污染。本发明工艺适用于连续大批量生产。The technical points of this invention are based on the composition characteristics and physical and chemical properties (good hydrophilicity and thermal stability) of bamboo leaf flavonoids, using ethanol aqueous solution for one-time heat reflux extraction; according to the flocculation and precipitation characteristics of impurities under certain conditions , use physical methods to separate and remove impurities; then use n-butanol to extract step by step, recover the solvent, and obtain the extract after being dissolved in water, and then dry to obtain the powder. The process is simple and easy to control; less investment in equipment, good separation effect, high extraction rate; no organic solvent residue, good quality of finished products; the whole process does not use toxic, harmful reagents and strong acid and alkali, basically no "three wastes" discharge, no pollution environmental pollution. The process of the invention is suitable for continuous mass production.
本发明使长期废弃的竹叶得到了深度开发,既实现了竹子的整株利用,由为社会提供了一种来源广阔、优质廉价的生物黄酮新资源,对人类的衰老、肿瘤和心血管病等退型性疾病的预防和治疗具有重要意义。The invention makes the long-term discarded bamboo leaves be deeply developed, not only realizes the utilization of the whole bamboo plant, but also provides a new bioflavonoid resource with a wide source, high quality and low price for the society, which is effective for human aging, tumors and cardiovascular diseases. The prevention and treatment of such degenerative diseases are of great significance.
竹叶总黄酮制备的工艺要点如下:The key points of the process for the preparation of total flavonoids from bamboo leaves are as follows:
(1)竹叶原料可以是散生竹或丛生竹的干青叶,以刚竹属的种类(如毛金竹、桂竹、毛竹、哺鸡竹、早园竹、高节竹、紫竹、斑竹等)为佳,理想的采收期是秋冬季(9~12月)。(1) Bamboo leaf raw materials can be dried green leaves of scattered bamboos or clustered bamboos, such as bamboos of the genus Phyllostachys osmanthus (such as Phyllostachys pubescens, Osmanthus osmanthus, Phyllostachys osmanthus, Phyllostachys osmanthus, Bamboo japonica, Bamboo japonica, Bamboo sargassum, Purple bamboo, Bamboo mosaic, etc. ) is better, and the ideal harvesting period is autumn and winter (September to December).
(2)一次性热回流提取。取干青叶的碎片,用1∶10~15料液比、20~40%浓度的乙醇溶液)热回流提取1~2hr,周期短、设备占用率低、提取较完全。鉴于竹叶原料的广泛性和低廉的价格,该一次性提取法是最经济、合理的方法。(2) One-time heat reflux extraction. Take the fragments of dried green leaves, and use 1:10-15 solid-liquid ratio, 20-40% concentration of ethanol solution) to extract by hot reflux for 1-2 hours, the cycle is short, the equipment occupancy rate is low, and the extraction is relatively complete. In view of the extensiveness and low price of bamboo leaf raw materials, this one-time extraction method is the most economical and reasonable method.
(3)物理法去杂。竹叶提取液浓缩到1∶1体积左右(即1kg干叶得1kg左右的浓缩液),在自然降温的静止过程中,内含的大分子杂质和部分多酚类成分发生絮凝,自然沉降,用离心分离、压滤或真空抽滤的方法除去,具有良好的澄清效果。该物理去杂法较之常规的醇沉或其他化学方法澄清,大大节省了生产成本,并且避免了化学试剂对提取物质量可能带来的不良影响。(3) Physical method to remove impurities. Bamboo leaf extract is concentrated to a volume of about 1:1 (that is, 1 kg of dry leaves gets about 1 kg of concentrated liquid). During the static process of natural cooling, the contained macromolecular impurities and some polyphenols will flocculate and settle naturally. It can be removed by centrifugation, pressure filtration or vacuum filtration, which has a good clarification effect. Compared with conventional alcohol precipitation or other chemical methods, this physical decontamination method greatly saves production costs and avoids possible adverse effects of chemical reagents on the quality of the extract.
(4)竹叶黄酮的精制采用正丁醇液~液萃取法。由于正丁醇对竹叶黄酮糖甙有很好的溶解性和选择性,加之其沸点较高、在室温下不易挥发,比重小、易于分离和回收,且无毒、无害。用正丁醇进行有效次数的萃取,黄酮提取率高,成品色泽金黄。(4) The refining of bamboo leaf flavonoids adopts n-butanol liquid-liquid extraction. Because n-butanol has good solubility and selectivity to bamboo leaf flavonoid glycosides, in addition, it has a high boiling point, is not volatile at room temperature, has a small specific gravity, is easy to separate and recover, and is non-toxic and harmless. Using n-butanol for effective times of extraction, the extraction rate of flavonoids is high, and the color of the finished product is golden.
(5)正丁醇萃取液经过减压浓缩、回收溶剂后,提取物再用少量的热水转溶成黄酮类化合物浸膏,再经真空干燥或喷雾干燥即得黄酮类化合物粉剂。(5) After the n-butanol extract is concentrated under reduced pressure and the solvent is recovered, the extract is transferred into a flavonoid extract with a small amount of hot water, and then vacuum-dried or spray-dried to obtain a flavonoid powder.
用本发明的技术制备的竹叶黄酮类化合物粉剂为黄色粉末或黄色结晶颗粒,带有明显的竹叶芳香,总黄酮含量在24~30%,绝大部分是黄酮糖苷,其中含相当数量的碳苷黄酮,如荭草苷木糖苷、异荭草苷和4’-甲氧基-牡荆苷等。其他成分还有植物酚酸、蒽醌、萜类内酯、含氮化合物、可溶性糖和矿物质等。The bamboo leaf flavonoid compound powder prepared by the technology of the present invention is yellow powder or yellow crystalline granules, with obvious bamboo leaf aroma, and the total flavonoid content is 24-30%, most of which are flavone glycosides, which contain a considerable amount of Carbon glycoside flavonoids, such as orientin xyloside, isoorientin and 4'-methoxy-vitexin, etc. Other ingredients include plant phenolic acids, anthraquinones, terpenoid lactones, nitrogenous compounds, soluble sugars and minerals.
实施例1:毛金竹(Phyllostachy nigra var.henonis(Bean)Stapf exRendle)的干青叶1kg,用破碎机破碎成10目左右的粗片后放入20L的提取罐中,加入30%的乙醇12kg,浸泡1hr,加热回流1.5hr。粗提液(约10kg)经过滤后入真空浓缩器中减压浓缩(同时回收溶剂),浓缩至体积为1L左右时出料,静止8hr,真空抽滤去除杂质,清液用同体积的正丁醇萃取三次(正丁醇预先用水饱和,40~50℃保温萃取、每次搅拌0.5~1hr),合并正丁醇相入真空浓缩器中减压浓缩回收溶剂,提取物用热水转溶,减压浓缩至一定浓度后成浸膏,或再经喷雾干燥得25g黄色粉末,其总黄酮含量为28%Embodiment 1: dry green leaf 1kg of Phyllostachy nigra var.henonis (Bean) Stapf exRendle), be broken into about 10 order coarse pieces with crusher and put into the extraction tank of 20L after, add 30% ethanol 12kg , Soak for 1hr, heat to reflux for 1.5hr. The crude extract (about 10kg) is filtered and concentrated in a vacuum concentrator under reduced pressure (recovering the solvent at the same time). When concentrated to a volume of about 1L, the material is discharged, rested for 8 hours, and vacuum filtered to remove impurities. Extract with butanol three times (pre-saturated n-butanol with water, extract at 40-50°C with heat preservation, and stir for 0.5-1 hr each time), combine the n-butanol phase into a vacuum concentrator to concentrate under reduced pressure to recover the solvent, and transfer the extract to hot water , concentrated under reduced pressure to a certain concentration to form an extract, or spray-dried to obtain 25g yellow powder, the total flavonoid content of which is 28%.
实施例2:2kg桂竹(Phyllostachy bambusoides Sieb.Et Zucc)的干青叶,破碎成10目左右的粗片放入50L的提取罐中,加入35%的乙醇30kg,浸泡0.5hr,加热回流1hr,提取液过滤后放入储罐中,用真空浓缩器分批浓缩至最终体积约为2L,静止6hr,离心分离去除杂质,清液用2倍体积的正丁醇萃取2次,合并正丁醇相,减压浓缩回收溶剂,提取物经热水转溶后,减压浓缩至比重大于1.12后成浸膏,或再经真空干燥得45g黄色粉末,总黄酮含量为27.6%。Embodiment 2: the dried green leaf of 2kg sweet-scented bamboo (Phyllostachy bamboosoides Sieb.Et Zucc), be broken into the thick sheet of about 10 orders and put into the extraction jar of 50L, add the ethanol 30kg of 35%, soak 0.5hr, reflux 1hr, After the extract is filtered, put it into a storage tank, concentrate in batches with a vacuum concentrator to a final volume of about 2L, let it stand for 6 hours, and centrifuge to remove impurities. The clear liquid is extracted twice with 2 times the volume of n-butanol, and the n-butanol phase, concentrated under reduced pressure to recover the solvent, and after the extract was trans-dissolved in hot water, concentrated under reduced pressure until the specific gravity was greater than 1.12 to form an extractum, or dried in vacuo to obtain 45g yellow powder with a total flavonoid content of 27.6%.
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