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CN1965915A - Method for extracting bitter buckwheat flavone in high purity - Google Patents

️Wed May 23 2007

CN1965915A - Method for extracting bitter buckwheat flavone in high purity - Google Patents

Method for extracting bitter buckwheat flavone in high purity Download PDF

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Publication number

CN1965915A

CN1965915A CNA2006101021477A CN200610102147A CN1965915A CN 1965915 A CN1965915 A CN 1965915A CN A2006101021477 A CNA2006101021477 A CN A2006101021477A CN 200610102147 A CN200610102147 A CN 200610102147A CN 1965915 A CN1965915 A CN 1965915A Authority

China

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solution

extract

purity

tartary buckwheat

reflux

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2006-11-11

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CNA2006101021477A

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CN100566728C (en

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李青山

周瑞雪

韩玲革

刘恩荔

梁泰刚

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Shanxi Medical University

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Shanxi Medical University

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2006-11-11

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2006-11-11

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2007-05-23

2006-11-11 Application filed by Shanxi Medical University filed Critical Shanxi Medical University

2006-11-11 Priority to CNB2006101021477A priority Critical patent/CN100566728C/en

2007-05-23 Publication of CN1965915A publication Critical patent/CN1965915A/en

2009-12-09 Application granted granted Critical

2009-12-09 Publication of CN100566728C publication Critical patent/CN100566728C/en

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2026-11-11 Anticipated expiration legal-status Critical

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Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

本发明涉及苦荞黄酮的提取方法，具体为一种高纯度苦荞黄酮的提取方法。本发明解决现有苦荞黄酮提取方法出膏率高、纯度低以及工艺流程比较复杂、生产成本较高等缺点。该提取方法包含苦荞种子经回流提取、浓缩制得浓缩液和浓缩液分离纯化；采用30％－80％的乙醇或甲醇或丙醇或乙酸乙酯溶液进行回流提取，回流提取液浓缩至苦荞种子重量与提取液的体积之比为1∶4－1∶6；浓缩液静置冷却，在15℃－30℃温度下，上离心机离心分离，弃去上清液，沉淀部分经干燥，即得到高纯度提取物。该提取方法工序减少，设备简单，生产成本低，产品稳定性增强，特别适合工业化生产。所得提取物不仅精制程度高，出膏率在3％以下，而且总黄酮纯度在50％以上。The invention relates to an extraction method of tartary buckwheat flavonoids, in particular to an extraction method of high-purity tartary buckwheat flavonoids. The invention solves the shortcomings of the existing tartary buckwheat flavonoid extraction method, such as high cream yield, low purity, complicated technical process and high production cost. The extraction method comprises the steps of extracting tartary buckwheat seeds under reflux, concentrating to obtain a concentrated solution, and separating and purifying the concentrated solution; using 30%-80% ethanol or methanol or propanol or ethyl acetate solution for reflux extraction, and reflux extracting solution is concentrated until bitter The ratio of the weight of buckwheat seeds to the volume of the extract is 1:4-1:6; the concentrated solution is left to cool, and is centrifuged in a centrifuge at a temperature of 15°C-30°C, the supernatant is discarded, and the precipitated part is dried , to obtain a high-purity extract. The extraction method has fewer procedures, simple equipment, low production cost and enhanced product stability, and is especially suitable for industrialized production. The obtained extract not only has a high degree of refinement, the cream yield is below 3%, and the purity of the total flavonoids is above 50%.

Description

一种高纯度苦荞黄酮的提取方法A kind of extraction method of high-purity tartary buckwheat flavonoids

技术领域technical field

本发明涉及苦荞黄酮的提取方法，具体为一种高纯度苦荞黄酮的提取方法。The invention relates to an extraction method of tartary buckwheat flavonoids, in particular to an extraction method of high-purity tartary buckwheat flavonoids.

背景技术Background technique

荞麦为双子叶蓼科荞麦属一年生植物，栽培的荞麦有两种类型：一种是普通荞麦，又称为甜荞(Fagopyrum esculentum)，子粒呈三棱形；另一种是鞑靼荞麦(Fagopymmt～aricum)，俗称苦荞，比普通荞麦粒小，棱角钝、粒色灰暗、无光泽、料面粗糙、皮层不易脱落。《本草纲目》记载：苦荞麦性味苦、平、寒、有益气力，续精神，利耳目，有降气宽肠健胃的作用。现代临床医学观察表明，荞麦具有降血糖、降血脂，增强人体免疫力的作用，对糖尿病、高血压、高血脂、冠心病、中风等病人都有辅助治疗作用。Buckwheat is an annual plant of the dicotyledonous Polygonaceae buckwheat. There are two types of cultivated buckwheat: one is common buckwheat, also known as sweet buckwheat (Fagopyrum esculentum), and its grain is triangular; the other is tartar buckwheat (Fagopyrum esculentum). ~aricum), commonly known as tartary buckwheat, is smaller than ordinary buckwheat grains, with blunt edges and corners, dark grain color, dull, rough material surface, and hard to fall off. "Compendium of Materia Medica" records: Tartary buckwheat has a bitter, flat, cold taste, is beneficial to energy, maintains spirit, benefits eyes and ears, and has the effect of lowering qi, widening intestines and strengthening stomach. Modern clinical medical observations show that buckwheat has the effects of lowering blood sugar and blood lipids, enhancing human immunity, and has adjuvant therapeutic effects on patients with diabetes, hypertension, hyperlipidemia, coronary heart disease, and stroke.

苦荞麦主要含黄酮类、氨基酸、有机酸类、多肽、蛋白质及镁、硒等微量元素。其中已知的黄酮类物质有芦丁、槲皮素、山奈酚、山奈酚-3-O-芸香糖苷等单一化合物。Tartary buckwheat mainly contains flavonoids, amino acids, organic acids, polypeptides, proteins and trace elements such as magnesium and selenium. The known flavonoids include single compounds such as rutin, quercetin, kaempferol, and kaempferol-3-O-rutinoside.

苦荞提取物——苦荞黄酮具有较强的生理活性，毒理学实验证明其为无毒、无副作用的物质，药效学的动物实验及临床观察表明其具有较显著的降血糖、降血脂、抗疲劳、增强免疫功能等作用。Tartary buckwheat extract - tartary buckwheat flavonoids have strong physiological activity. Toxicology experiments have proved that they are non-toxic and have no side effects. Pharmacodynamic animal experiments and clinical observations have shown that they have more significant hypoglycemic and blood lipid , anti-fatigue, enhance immune function and so on.

目前市场上以苦荞为原料的品种多为粗加工制品如：“苦荞系列保健食品一绿粒宝”(发明专利，公开号CN 1101238A)，“苦荞降糖粉及其制备方法”(发明专利，公开号CN 1363230A)。而对苦荞有效成分进一步精制纯化，使其能够符合现代制剂“三效”、“三小”(高效、速效、长效和剂量小、毒性小、副作用小)的要求是其实现中药现代化的必然趋势；目前中药材的常规提取物制备主要是运用水煎法、碱溶酸沉法、有机溶媒法、大孔树脂法等方法，这些提取方法制得的提取物常具有吸湿性较大、出膏率较高、服用量大、黄酮类物质纯度较低、黄酮类物质中有效成分相对单一(仅包含一种或几种化合物)、工艺流程比较复杂、生产成本较高等缺点；采用现有的提取技术来提取苦荞黄酮，其出膏率一般在10％左右，提取物中黄酮类物质含量较低，但要得到高纯度的苦荞提取物(黄酮类物质含量50％以上)，出膏率控制在3％以下，又不降低有效成分含量就很难了。这里出膏率(如3％)是指单位干燥药材质量(如100g药材)制备获得的最终干燥提取物的质量(如3g)。出膏率越小，表明提取物精制程度越高；但是只有出膏率还不行，因为如果制备的提取物不含活性成分，则出膏率越小，有可能药理活性会越小。Currently on the market, the varieties of tartary buckwheat as raw materials are mostly rough-processed products such as: "Tartary Buckwheat Series Health Food-Lvlibao" (invention patent, publication number CN 1101238A), "Tartary Buckwheat Hydrating Sugar Powder and Its Preparation Method" ( Invention patent, publication number CN 1363230A). The further refinement and purification of the active ingredients of tartary buckwheat, so that it can meet the requirements of modern preparations "three effects" and "three small" (high efficiency, quick effect, long effect, small dose, low toxicity, and small side effects) is the modernization of traditional Chinese medicine. Inevitable trend; at present, the conventional extracts of traditional Chinese medicinal materials are mainly prepared by decocting in water, alkali-soluble acid precipitation, organic solvents, and macroporous resins. The extracts obtained by these extraction methods often have high hygroscopicity, Disadvantages such as high cream yield, large dosage, low purity of flavonoids, relatively single active ingredient in flavonoids (only containing one or several compounds), complicated process, high production cost, etc.; Tartary buckwheat flavonoids are extracted by advanced extraction technology, the yield is generally about 10%, and the content of flavonoids in the extract is low, but to obtain high-purity tartary buckwheat extract (flavonoid content is more than 50%), the output It is difficult to control the paste rate below 3% without reducing the active ingredient content. The paste yield (eg, 3%) here refers to the mass (eg, 3 g) of the final dry extract prepared by the unit mass of dried medicinal material (eg, 100 g of medicinal material). The smaller the cream yield, the higher the refining degree of the extract; but only the cream yield is not enough, because if the prepared extract does not contain active ingredients, the smaller the cream yield, the lower the pharmacological activity may be.

目前未见出膏率在3％以下，黄酮类物质纯度达50％以上苦荞总黄酮提取方法的报道。At present, there is no report on the extracting method of tartary buckwheat total flavonoids with a cream yield below 3% and a flavonoid purity of more than 50%.

发明内容Contents of the invention

本发明为了解决现有苦荞黄酮提取方法出膏率高、纯度低以及工艺流程比较复杂、生产成本较高等缺点，提供一种新的苦荞黄酮的提取方法——一种高纯度苦荞黄酮的提取方法。The present invention provides a new extraction method of tartary buckwheat flavonoids—a high-purity tartary buckwheat flavonoids in order to solve the shortcomings of the existing tartary buckwheat flavonoids extraction method, such as high cream yield, low purity, complex process flow, and high production cost. extraction method.

本发明是采用如下技术方案实现的：一种高纯度苦荞黄酮的提取方法，包含苦荞种子经回流提取、浓缩制得浓缩液和浓缩液分离纯化；采用30％-80％的乙醇或甲醇或丙醇或乙酸乙酯溶液进行回流提取，回流提取液浓缩至苦荞种子重量(克)与提取液的体积(毫升)之比为1∶4-1∶6；浓缩液静置冷却，在15℃-30℃温度下，上离心机离心分离，弃去上清液，沉淀部分经干燥，即得到高纯度提取物。回流提取溶液及其浓度的选择最终决定提取物的出膏率和黄酮类物质的纯度；本发明所用回流提取溶液(乙醇或甲醇或丙醇或乙酸乙酯溶液)及其浓度(30％-80％)保证了苦荞种子中的大部分有效成分溶于提取液中，避免了大部分的无效成分(如淀粉等)溶于提取液，从而保证提取物有低的出膏率(3％以下)和高纯度的黄酮类物质(50％以上)。提取液的浓缩程度决定后续离心分离纯化的效果，浓缩液过稀(即苦荞种子重量与提取液的体积之比过小)，浓缩液中的有效物质(包括黄酮类物质)不能充分地离心分离出来，部分有效物质会留于浓缩液中，从而影响出膏率(在3％以下的范围内)和黄酮类物质的纯度，浓缩液过浓(即苦荞种子重量与提取液的体积之比过大)，浓缩液会在容器内壁形成挂壁，从而损失有效物质，也会影响出膏率(在3％以下的范围内)和黄酮类物质的纯度。离心温度是分离纯化的一个重要参数，离心温度不合适将极大地影响提取物的黄酮纯度。本发明通过大量实验确定的离心温度(15℃-30℃)能充分保证提取物中的黄酮纯度在50％以上。The present invention is realized by adopting the following technical scheme: a method for extracting high-purity tartary buckwheat flavonoids, comprising extracting and concentrating tartary buckwheat seeds to obtain a concentrated solution and separating and purifying the concentrated solution; using 30%-80% ethanol or methanol or propanol or ethyl acetate solution for reflux extraction, and the reflux extract is concentrated to a ratio of buckwheat seed weight (grams) to the volume (milliliters) of the extract is 1: 4-1: 6; Centrifuge in a centrifuge at a temperature of 15°C-30°C, discard the supernatant, and dry the precipitated part to obtain a high-purity extract. The selection of reflux extraction solution and its concentration finally determines the yield of the extract and the purity of flavonoids; the reflux extraction solution (ethanol or methyl alcohol or propanol or ethyl acetate solution) and its concentration (30%-80 %) ensured that most of the active ingredients in the tartary buckwheat seeds were dissolved in the extract, and avoided that most of the ineffective ingredients (such as starch, etc.) were dissolved in the extract, thereby ensuring that the extract had a low cream yield (less than 3%) ) and high-purity flavonoids (more than 50%). The degree of concentration of the extract determines the effect of subsequent centrifugal separation and purification. If the concentrate is too dilute (that is, the ratio of the weight of buckwheat seeds to the volume of the extract is too small), the effective substances (including flavonoids) in the concentrate cannot be centrifuged sufficiently. Separated, some effective substances will stay in the concentrated solution, thereby affecting the paste yield (in the scope of less than 3%) and the purity of flavonoids, and the concentrated solution is too thick (the difference between the weight of tartary buckwheat seeds and the volume of the extract) ratio is too large), the concentrated solution will form a wall on the inner wall of the container, thereby losing the effective substance, and also affecting the paste yield (in the range below 3%) and the purity of the flavonoids. Centrifugation temperature is an important parameter for separation and purification, and improper centrifugation temperature will greatly affect the purity of flavonoids in the extract. The centrifugation temperature (15°C-30°C) determined through a large number of experiments in the present invention can fully ensure that the flavonoid purity in the extract is above 50%.

本发明选用的离心机转速为不小于5000r·min^-1，离心时间不小于15min。在该离心机参数下，可保证浓缩液中的有效物质基本离心分离出来，并保证提取物的黄酮纯度在50％以上。离心机转速过低、离心时间过短，无法保证提取液中的有效物质充分分离出来，无法保证应有的出膏率和黄酮纯度；当然大于5000r·min^-1的离心机转速和超过15min的离心时间，出膏率会在不超过3％的范围内略有提高(离心机转速再高、离心时间再长，出膏率也不会超过3％，因为出膏率的最终量已经由提取液的制备决定了)，黄酮纯度也会略有提高，从而在一定程度上提高提取得率，但离心机要耗费更多的能源，这里存在一个权衡利弊的问题。本发明选用的离心机转速为不小于5000r·min^-1，离心时间不小于15min是保证提取物具有较理想出膏率和黄酮纯度达到50％以上的低限。The rotation speed of the centrifuge selected in the present invention is not less than 5000r·min ^-1 , and the centrifugation time is not less than 15min. Under the parameters of the centrifuge, it can ensure that the effective substances in the concentrated solution are basically centrifuged and separated, and the flavonoid purity of the extract is guaranteed to be above 50%. The speed of the centrifuge is too low and the centrifugation time is too short to ensure that the effective substances in the extract are fully separated, and the proper cream yield and flavonoid purity cannot be guaranteed; of course, the speed of the centrifuge is greater than ^5000r ·min The centrifugation time, the paste yield will be slightly increased within the range of no more than 3% (no matter how high the centrifuge speed is, and no matter how long the centrifugation time is, the paste yield will not exceed 3%, because the final amount of the paste yield has been extracted. The preparation of the solution is determined), the purity of flavonoids will also be slightly improved, thereby improving the extraction yield to a certain extent, but the centrifuge will consume more energy, and there is a problem of weighing the pros and cons here. The rotation speed of the centrifuge selected in the present invention is not less than 5000r·min ^-1 , and the centrifugation time is not less than 15min to ensure that the extract has a relatively ideal cream yield and the flavonoid purity reaches the lower limit of more than 50%.

提取溶液浓度在30％-80％的范围内可进一步优化，以获得更佳的提取效果。提取溶液浓度可选择30％-70％、30％-60％、40％-80％、40％-70％、50％-70％、60％-70％。甲醇相对毒性较大。丙酮成本较高。本发明优选乙醇溶液作为回流提取溶液，并优选50％-70％的乙醇溶液作为回流提取溶液，以获得进一步优化的提取效果。提取液的浓缩可采用减压浓缩、薄膜浓缩等方法；提取物的干燥可采用常压烘干、减压干燥、喷雾干燥和冷冻干燥等技术。这些方法均是本领域内的公知公用的方法。The concentration of the extraction solution can be further optimized in the range of 30%-80% to obtain a better extraction effect. The concentration of the extraction solution can be selected from 30%-70%, 30%-60%, 40%-80%, 40%-70%, 50%-70%, 60%-70%. Methanol is relatively toxic. Acetone is expensive. In the present invention, ethanol solution is preferably used as the reflux extraction solution, and preferably 50%-70% ethanol solution is used as the reflux extraction solution, so as to obtain a further optimized extraction effect. The concentration of the extract can be concentrated under reduced pressure, thin film concentration and other methods; the drying of the extract can be dried under normal pressure, vacuum drying, spray drying and freeze drying. These methods are all well-known and public methods in the art.

本发明所述的高纯度苦荞黄酮的提取方法与传统方法相比，工序减少，生产周期缩短，设备简单，生产成本低，产品稳定性增强，特别适合工业化生产。以本发明所述方法得到的提取物不仅精制程度高，出膏率在3％以下，而且保留了大部分苦荞的活性成分-总黄酮，总黄酮纯度在50％以上，使服用量远小于苦荞粗提物，具有现代中药“三小”、“三效”的特点。因此本发明提供的苦荞高纯提取物作为药用组合物能够用于治疗或预防糖尿病及其并发症。本发明所述提取方法对于更加有效的利用苦荞植物资源，拓宽苦荞植物的应用也具有重要意义。Compared with the traditional method, the extraction method of the high-purity tartary buckwheat flavonoids of the present invention has fewer procedures, shortened production cycle, simple equipment, low production cost and enhanced product stability, and is especially suitable for industrial production. The extract obtained by the method of the present invention not only has a high degree of refinement, and the cream yield is below 3%, but also retains most of the active ingredients of tartary buckwheat - total flavonoids, and the purity of total flavonoids is above 50%, so that the dosage is far less than Tartary buckwheat crude extract has the characteristics of "three small" and "three effects" of modern Chinese medicine. Therefore, the high-purity tartary buckwheat extract provided by the invention can be used as a pharmaceutical composition for treating or preventing diabetes and its complications. The extraction method of the invention is also of great significance for more effectively utilizing tartary buckwheat plant resources and broadening the application of tartary buckwheat plants.

具体实施方式Detailed ways

实施例1Example 1

1.提取1. Extraction

取苦荞原药材(干燥种子100g)。提取前可经干燥或烘干处理。其中苦荞是指双子叶蓼科荞麦属植物。在85℃-100℃的温度下，以1000mL的60％(或30％或40％或45％或50％或55％或60％或65％或70％或80％)乙醇水回流提取3次(1000mL×3)，每次2hr，合并提取液，滤过，滤液减压浓缩(60℃，0.08-0.1MPa)，至总体积约500mL，室温静置2-4hr，采用高速离心机或普通离心机，将样品在15℃～30℃下(15℃、20℃、25℃、30℃)，离心转速5000r·min^-1，离心时间为15min的条件下将浓缩液离心，弃去上清液，将沉淀置水浴蒸干后，50℃～75℃烤箱干燥2～72hr，得黄棕色至黄色粉末，为苦荞高纯提取物，总量为2.22g。出膏率为2.22％。Get the original medicinal material of tartary buckwheat (dried seeds 100g). It can be dried or dried before extraction. Wherein tartary buckwheat refers to the dicotyledonous Polygonaceae buckwheat plant. At a temperature of 85°C-100°C, reflux extraction with 1000mL of 60% (or 30% or 40% or 45% or 50% or 55% or 60% or 65% or 70% or 80%) ethanol water for 3 times (1000mL×3), 2hr each time, combine the extracts, filter, and concentrate the filtrate under reduced pressure (60°C, 0.08-0.1MPa) to a total volume of about 500mL, stand at room temperature for 2-4hr, use a high-speed centrifuge or ordinary Centrifuge, centrifuge the sample at 15°C-30°C (15°C, 20°C, 25°C, 30°C), centrifuge at a speed of 5000r·min ^-1 , centrifuge for 15min, and discard the supernatant After the precipitate was evaporated to dryness in a water bath, it was oven-dried at 50°C to 75°C for 2 to 72 hours to obtain a yellowish brown to yellow powder, which was a high-purity tartary buckwheat extract, with a total amount of 2.22g. The paste yield was 2.22%.

2.总黄酮的含量测定：2. Determination of the content of total flavonoids:

对照品溶液制备：精密称取芦丁对照品适量，用60％乙醇配置成1ml含92.8μg的溶液，供试品溶液制备；Preparation of reference substance solution: accurately weigh an appropriate amount of rutin reference substance, configure 1ml of a solution containing 92.8 μg with 60% ethanol, and prepare the test solution;

精密称取干燥本品0.05g，置于50mL量瓶中，加入60％乙醇溶液溶解，定容至刻度，称重，超声溶解，补足重量，备用。Accurately weigh 0.05g of this dry product, place it in a 50mL measuring bottle, add 60% ethanol solution to dissolve, set the volume to the mark, weigh, dissolve with ultrasound, make up the weight, and set aside.

测定方法：取对照品溶液及供试品溶液，置10mL容量瓶中，加入AlCl₃和KAc，用60％乙醇加至10mL，显色30min，按分光光度法(中国药典2000版附录IVA)，在418nm处测定吸光度，测得本实施例总黄酮物质含量为55.44％。Assay method: get reference substance solution and need testing solution, put in 10mL volumetric flask, add AlCl ₃ and KAc, add to 10mL with 60% ethanol, develop color 30min, press spectrophotometry (2000 edition appendix IVA of Chinese Pharmacopoeia), The absorbance was measured at 418nm, and the total flavonoid content in this example was measured to be 55.44%.

实施例2Example 2

1.提取1. Extraction

取苦荞原药材(干燥种子100g)。提取前可经干燥或烘干处理。其中苦荞是指双子叶蓼科荞麦属植物。在85℃-100℃的温度下，以1000mL的50％(或30％或40％或45％或55％或60％或65％或70％或80％)甲醇水回流提取3次(1000mL×3)，每次2hr，合并提取液，滤过，滤液减压浓缩(60℃，0.08-0.1MPa)，至总体积约600mL，室温静置2-4hr，采用高速离心机或普通离心机，将样品在15℃～30℃下(15℃、20℃、25℃、30℃)，离心转速8000r·min^-1，离心时间为30min的条件下将浓缩液离心，弃去上清液，将沉淀置水浴蒸干后，50℃～75℃烤箱干燥2～72hr，得黄棕色至黄色粉末，为苦荞高纯提取物，总量为2.52g。出膏率为2.52％。Get the original medicinal material of tartary buckwheat (dried seeds 100g). It can be dried or dried before extraction. Wherein tartary buckwheat refers to the dicotyledonous Polygonaceae buckwheat plant. At a temperature of 85°C-100°C, reflux extraction with 1000mL of 50% (or 30% or 40% or 45% or 55% or 60% or 65% or 70% or 80%) methanol water for 3 times (1000mL× 3), 2 hours each time, combine the extracts, filter, and concentrate the filtrate under reduced pressure (60°C, 0.08-0.1MPa) to a total volume of about 600mL, let stand at room temperature for 2-4hrs, use a high-speed centrifuge or an ordinary centrifuge, Centrifuge the sample at 15°C-30°C (15°C, 20°C, 25°C, 30°C), centrifuge at a speed of 8000r·min ^-1 , and centrifuge for 30min, discard the supernatant, and After the precipitate was evaporated to dryness in a water bath, it was oven-dried at 50°C to 75°C for 2 to 72 hours to obtain a yellowish brown to yellow powder, which was a high-purity tartary buckwheat extract, with a total amount of 2.52g. The paste yield was 2.52%.

2.总黄酮的含量测定：2. Determination of the content of total flavonoids:

测定方法：取对照品溶液及供试品溶液，置10mL容量瓶中，加入AlCl₃和KAc，用60％乙醇加至10mL，显色30min，按分光光度法(中国药典2000版附录IVA)，在418nm处测定吸光度，测得本实施例总黄酮物质含量为55.74％。Assay method: get reference substance solution and need testing solution, put in 10mL volumetric flask, add AlCl ₃ and KAc, add to 10mL with 60% ethanol, develop color 30min, press spectrophotometry (2000 edition appendix IVA of Chinese Pharmacopoeia), The absorbance was measured at 418nm, and the total flavonoid content in this example was measured to be 55.74%.

实施例3Example 3

1.提取1. Extraction

取苦荞原药材(干燥种子100g)。提取前可经干燥或烘干处理。其中苦荞是指双子叶蓼科荞麦属植物。在85℃-100℃的温度下，以1000mL的70％(或30％或40％或45％或50％或55％或60％或65％或80％)丙酮水回流提取3次(1000mL×3)，每次2hr，合并提取液，滤过，滤液减压浓缩(60℃，0.08-0.1MPa)，至总体积约400mL，室温静置2-4hr，采用高速离心机或普通离心机，将样品在15℃～30℃下(15℃、20℃、25℃、30℃)，离心转速13000r·min^-1，离心时间为65min的条件下将浓缩液离心，弃去上清液，将沉淀置水浴蒸干后，50℃～75℃烤箱干燥2～72hr，得黄棕色至黄色粉末，为苦荞高纯提取物，总量为2.82g。出膏率为2.82％。Get the original medicinal material of tartary buckwheat (dried seeds 100g). It can be dried or dried before extraction. Wherein tartary buckwheat refers to the dicotyledonous Polygonaceae buckwheat plant. At a temperature of 85°C-100°C, reflux extraction with 1000mL of 70% (or 30% or 40% or 45% or 50% or 55% or 60% or 65% or 80%) acetone water for 3 times (1000mL× 3), 2 hours each time, combine the extracts, filter, and concentrate the filtrate under reduced pressure (60°C, 0.08-0.1MPa) to a total volume of about 400mL, and let it stand at room temperature for 2-4hrs, using a high-speed centrifuge or an ordinary centrifuge, The sample was centrifuged at 15°C-30°C (15°C, 20°C, 25°C, 30°C), with a centrifugation speed of 13000r·min ^-1 and a centrifugation time of 65min, and the supernatant was discarded. After the precipitate was evaporated to dryness in a water bath, it was oven-dried at 50°C to 75°C for 2 to 72 hours to obtain a yellowish brown to yellow powder, which was a high-purity tartary buckwheat extract, with a total amount of 2.82g. The paste yield was 2.82%.

2.总黄酮的含量测定：2. Determination of the content of total flavonoids:

测定方法：取对照品溶液及供试品溶液，置10mL容量瓶中，加入AlCl₃和KAc，用60％乙醇加至10mL，显色30min，按分光光度法(中国药典2000版附录IVA)，在418nm处测定吸光度，测得本实施例总黄酮物质含量为55.98％。Assay method: get reference substance solution and need testing solution, put in 10mL volumetric flask, add AlCl ₃ and KAc, add to 10mL with 60% ethanol, develop color 30min, press spectrophotometry (2000 edition appendix IVA of Chinese Pharmacopoeia), The absorbance was measured at 418nm, and the total flavonoid content in this example was measured to be 55.98%.

Claims (4)

1, a kind of extracting method of bitter buckwheat flavone in high purity, comprise the Radix Et Rhizoma Fagopyri Tatarici seed through reflux, extract,, concentrate and to make concentrated solution and concentrated solution separation and purification; It is characterized by: adopt the ethanol of 30%-80% or methanol or propanol or ethyl acetate solution to carry out reflux, extract,, the ratio that reflux extracting liquid is concentrated into Radix Et Rhizoma Fagopyri Tatarici seed weight and the volume of extracting solution is 1: 4-1: 6; Concentrated solution leaves standstill cooling, under 15 ℃ of-30 ℃ of temperature, and last centrifuge centrifugalize, abandoning supernatant, precipitation part drying promptly obtains the high-purity extract.

2, the extracting method of a kind of bitter buckwheat flavone in high purity as claimed in claim 1 is characterized by: centrifuge speed is for being not less than 5000rmin ^-1, centrifugation time is not less than 15min.

3, the extracting method of a kind of bitter buckwheat flavone in high purity as claimed in claim 1 or 2 is characterized by: the alcoholic solution that adopts 50%-70% is as reflux, extract, solution.

4, the extracting method of a kind of bitter buckwheat flavone in high purity as claimed in claim 3 is characterized by: the alcoholic solution of employing 60% is as reflux, extract, solution.

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Cited By (8)

* Cited by examiner, † Cited by third party

Publication number	Priority date	Publication date	Assignee	Title
CN101519457B (en) *	2009-03-17	2011-04-13	徐德平	Method for preparing beta-ethoxy rutinose and application thereof for reducing blood glucose
CN102861135A (en) *	2012-10-01	2013-01-09	师宗彤野食品有限公司	Extraction method of buckwheat flavonoids
CN102895323A (en) *	2012-10-11	2013-01-30	宁波杭州湾新区第九区科技服务有限公司	Method for extracting buckwheat flavonoid
CN103040951A (en) *	2012-09-07	2013-04-17	赵立地	Method for extracting buckwheat flavonoids
CN103829123A (en) *	2014-01-09	2014-06-04	山西春阳生物科技有限公司	Method for producing hypoglycemic hypolipemic product by using tartary buckwheat
CN103829122A (en) *	2014-01-09	2014-06-04	山西春阳生物科技有限公司	Production method of capsule rich in beta-ethoxy rutinose
CN104069187A (en) *	2014-07-24	2014-10-01	劲牌生物医药有限公司	Technological method extracting duckwheat flavone from duckwheat
CN107913309A (en) *	2017-11-28	2018-04-17	张夏洋	The method of the total brass of high efficiency extraction bitter buckwheat seed

2006
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Cited By (9)

* Cited by examiner, † Cited by third party

Publication number	Priority date	Publication date	Assignee	Title
CN101519457B (en) *	2009-03-17	2011-04-13	徐德平	Method for preparing beta-ethoxy rutinose and application thereof for reducing blood glucose
CN103040951A (en) *	2012-09-07	2013-04-17	赵立地	Method for extracting buckwheat flavonoids
CN102861135A (en) *	2012-10-01	2013-01-09	师宗彤野食品有限公司	Extraction method of buckwheat flavonoids
CN102861135B (en) *	2012-10-01	2014-05-28	师宗彤野食品有限公司	Extraction method of buckwheat flavonoids
CN102895323A (en) *	2012-10-11	2013-01-30	宁波杭州湾新区第九区科技服务有限公司	Method for extracting buckwheat flavonoid
CN103829123A (en) *	2014-01-09	2014-06-04	山西春阳生物科技有限公司	Method for producing hypoglycemic hypolipemic product by using tartary buckwheat
CN103829122A (en) *	2014-01-09	2014-06-04	山西春阳生物科技有限公司	Production method of capsule rich in beta-ethoxy rutinose
CN104069187A (en) *	2014-07-24	2014-10-01	劲牌生物医药有限公司	Technological method extracting duckwheat flavone from duckwheat
CN107913309A (en) *	2017-11-28	2018-04-17	张夏洋	The method of the total brass of high efficiency extraction bitter buckwheat seed

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CN1965915A - Method for extracting bitter buckwheat flavone in high purity - Google Patents