CN107126452A - Gypenosides and preparation method thereof - Google Patents
Gypenosides and preparation method thereof Download PDFInfo
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- CN107126452A CN107126452A CN201610106326.1A CN201610106326A CN107126452A CN 107126452 A CN107126452 A CN 107126452A CN 201610106326 A CN201610106326 A CN 201610106326A CN 107126452 A CN107126452 A CN 107126452A
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- 229930187479 gypenoside Natural products 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- FBFMBWCLBGQEBU-RXMALORBSA-N (2s,3r,4s,5s,6r)-2-[(2r,3r,4s,5s,6r)-2-[[(3s,5r,6s,8r,9r,10r,12r,13r,14r,17s)-3,12-dihydroxy-4,4,8,10,14-pentamethyl-17-[(2s)-6-methyl-2-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyhept-5-en-2-yl]-2,3,5,6,7,9,11,12,13,15,16,17-dodecah Chemical class O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O FBFMBWCLBGQEBU-RXMALORBSA-N 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 235000002956 Gynostemma pentaphyllum Nutrition 0.000 claims abstract description 47
- 240000006509 Gynostemma pentaphyllum Species 0.000 claims abstract description 32
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- JJURGRVZASRDDE-UHFFFAOYSA-N 17-[2,3-dihydroxy-5-(2-methylprop-1-enyl)oxolan-3-yl]-3-[5-hydroxy-3-(3,4,5-trihydroxy-6-methyloxan-2-yl)oxy-4-(3,4,5-trihydroxyoxan-2-yl)oxyoxan-2-yl]oxy-4,4,8,14-tetramethyl-2,3,5,6,7,9,11,12,13,15,16,17-dodecahydro-1H-cyclopenta[a]phenanthrene-10-carbaldehyde Chemical compound CC1OC(OC2C(OC3CCC4(C=O)C(CCC5(C)C4CCC4C(CCC54C)C4(O)CC(OC4O)C=C(C)C)C3(C)C)OCC(O)C2OC2OCC(O)C(O)C2O)C(O)C(O)C1O JJURGRVZASRDDE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/42—Cucurbitaceae (Cucumber family)
- A61K36/424—Gynostemma
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
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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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
本发明涉及一种绞股蓝总皂苷及其制备方法。属中药领域，涉及中药有效部位及其提取、纯化及精制方法，具体指一种从绞股蓝全草原料中提取精制绞股蓝皂苷及其制备方法。本发明将绞股蓝药材置于回流提取器中用高浓度乙醇进行回流提取，滤过，除醇得无醇滤液，滤液用大孔树脂进行吸附洗脱，洗脱液分别为水，低浓度碱，低浓度醇和高浓度醇，逐步洗脱后，得各洗脱液，保留高浓度醇洗脱液，浓缩蒸干，即得绞股蓝总皂苷。制得的绞股蓝总皂采用紫外分光光度法测定其中的总皂苷含量以绞股蓝皂苷A计，含量为92%~94%。本发明方法效率高，步骤简化，周期短，成本低，适用于工业化生产。The invention relates to a total gypenoside and a preparation method thereof. The invention belongs to the field of traditional Chinese medicines, and relates to effective parts of traditional Chinese medicines and methods for extracting, purifying and refining them, and specifically refers to a method for extracting and refining gypenosides from the whole herb of Gynostemma pentaphyllum and a preparation method thereof. In the present invention, the Gynostemma pentaphylla medicinal material is placed in a reflux extractor and extracted with high-concentration ethanol, filtered, and alcohol-free filtrate is obtained, and the filtrate is adsorbed and eluted with a macroporous resin, and the eluents are water, low-concentration alkali, respectively. After the low-concentration alcohol and high-concentration alcohol are eluted step by step, each eluent is obtained, and the high-concentration alcohol eluent is retained, concentrated and evaporated to dryness to obtain the total saponins of Gynostemma pentaphyllum. The total saponin content of the prepared Gynostemma pentaphyllum saponin is measured by ultraviolet spectrophotometry, and the content is 92% to 94% in terms of Gypenoside A. The method of the invention has high efficiency, simplified steps, short period and low cost, and is suitable for industrialized production.
Description
技术领域technical field
本发明属中药领域，涉及中药有效部位及其提取、纯化及精制方法，具体指一种从绞股蓝全草原料中提取精制绞股蓝皂苷及其制备方法。The invention belongs to the field of traditional Chinese medicines, and relates to effective parts of traditional Chinese medicines and methods for extracting, purifying and refining them, in particular to a method for extracting and refining gypenosides from gynostemma pentaphylla whole herb raw materials and a preparation method thereof.
背景技术Background technique
现有技术公开了绞股蓝为葫芦科绞股蓝属多年生攀援草本植物，又称七叶胆、五叶参、公罗锅底、落地生根和七叶参等，拉丁文名为Gynostemmapentaphyllum (Thunb.)Makino。该植物共分 13 种，分布于我国、日本和朝鲜及东南亚各国，其中，据调查显示，在我国有 11 种存在，即：单叶绞股蓝、光叶绞股蓝、缅甸绞股蓝、毛绞股蓝、长梗绞股蓝、啄果绞股蓝、心籽绞股蓝、小籽绞股蓝、聚果绞股蓝、疏花绞股蓝；其味苦、性甘寒、无毒，具有清热解毒、补气生津、祛痰止咳、安神固精的作用，主治慢性支气管炎、咳嗽、气喘、传染性肝炎，肾盂肾炎，以及健忘失眠、倦怠少食、梦遗滑精等症。The prior art discloses that Gynostemma pentaphyllum is a perennial climbing herb of Cucurbitaceae Gynostemma pentaphyllum, also known as Aescin, five-leaved ginseng, public Luoguodi, ground root and Aescin, etc., and its Latin name is Gynostemmapentaphyllum (Thunb.) Makino. The plant is divided into 13 species, which are distributed in my country, Japan, North Korea and Southeast Asian countries. Among them, according to the survey, there are 11 species in our country, namely: Gynostemma unileaf, Gynostemma light-leaf, Gynostemma burma, Gynostemma wool, and Gynostemma long-stemmed , Gynostemma pecking fruit, core seed Gynostemma, small seed Gynostemma, fruit-gathering Gynostemma, thinning Gynostemma; its taste is bitter, sweet and cold, non-toxic, and has the functions of clearing heat and detoxifying, invigorating qi and promoting body fluid, eliminating phlegm and relieving cough, calming the nerves and strengthening essence. Indications for chronic bronchitis, cough, asthma, infectious hepatitis, pyelonephritis, forgetfulness and insomnia, fatigue and lack of food, nocturnal emission and other diseases.
研究显示，绞股蓝植物中 含有皂苷类物质、黄酮类物质、多糖类物质、维生素类物质、菇类类物质、有机酸类物质、生物碱类物质、蛋白质类物质等有效成分。皂苷类物质是其主要成分之一，绞股蓝皂苷含有人参皂苷相同的四环三萜达玛烷型结构。绞股蓝中皂苷含量比较丰富，目前有关研究已先后从绞股蓝中分离鉴定了 80 余种皂苷。研究显示，绞股蓝皂苷具有降血脂、降胆固醇、降血压、增强冠状动脉和脑血流量、抗DNA的变异作用、提高机体免疫功能等作用。Studies have shown that Gynostemma Gynostemma contains active ingredients such as saponins, flavonoids, polysaccharides, vitamins, mushrooms, organic acids, alkaloids, and proteins. Saponins are one of its main components. Gypenoside contains the same tetracyclic triterpene dammarane structure as ginsenoside. The content of saponins in Gynostemma pentaphyllum is relatively rich. At present, relevant research has isolated and identified more than 80 kinds of saponins from Gynostemma pentaphyllum. Studies have shown that gypenoside has the functions of lowering blood fat, lowering cholesterol, lowering blood pressure, enhancing coronary artery and cerebral blood flow, anti-DNA variation, and improving immune function of the body.
目前， 从绞股蓝药材中提取皂苷类物质的常规提取方法有加水煎煮法、有机溶剂回流提取法、渗漉法等，以及有微波提取、超声提取法、酶辅助提取等各种新技术；但其中的精制的方法不多，主要利用皂苷类物质在正丁醇中溶解度大的特性，用正丁醇萃取，但正丁醇沸点高，回收不容易，且在终产物中残留量较大，工业化生产不易。At present, the conventional extraction methods for extracting saponins from Gynostemma pentaphyllum medicinal materials include decoction with water, organic solvent reflux extraction, percolation, etc., as well as various new technologies such as microwave extraction, ultrasonic extraction, and enzyme-assisted extraction; but There are not many refining methods, mainly using the characteristics of high solubility of saponins in n-butanol, and extracting with n-butanol, but n-butanol has a high boiling point, recovery is not easy, and the residual amount in the final product is relatively large. Industrial production is not easy.
基于现有技术的现状，本申请的发明人拟提供一种中药有效部位及其提取、纯化及精制的方法，尤其是从绞股蓝全草原料中提取精制绞股蓝皂苷及其制备方法。该方法将对工业化大生产提取精制绞股蓝皂苷具有现实意义。Based on the current state of the art, the inventor of the present application intends to provide a method for extracting, purifying and refining effective parts of traditional Chinese medicines, especially extracting and refining gypenoside from the whole herb of Gynostemma pentaphyllum and its preparation method. The method will have practical significance for the extraction of refined gypenoside in industrialized large-scale production.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种中药有效部位及其提取、纯化及精制的方法，具体涉及绞股蓝总皂苷及其制备方法，尤其是一种可工业化生产，成本低，工艺流程短的从绞股蓝中提取纯化绞股蓝总皂苷的方法。The technical problem to be solved by the present invention is to provide a method for extracting, purifying and refining the effective part of traditional Chinese medicine, specifically related to total saponins of Gypenoside and its preparation method, especially a kind of gypenoside that can be industrialized, has low cost and short process flow. A method for extracting and purifying total saponins of Gynostemma pentaphyllum from Gynostemma pentaphyllum.
本发明解决上述技术问题所采用的技术方案为，基于大孔吸附树脂是一类不含交换基团且有大孔结构的高分子吸附树脂，具有良好的大孔网状结构和较大的比表面积，以及，大孔吸附树脂越来越多的应用于中药与天然药物有效成分、有效部位的纯化和分离，且，所述的大孔吸附树脂可再生重复使用，生产成本低的特点，提供了一种从绞股蓝中提取精制绞股蓝皂苷的方法，其特征在于：包括如下步骤：The technical solution adopted by the present invention to solve the above-mentioned technical problems is that based on the fact that the macroporous adsorption resin is a kind of macromolecular adsorption resin that does not contain exchange groups and has a macroporous structure, it has a good macroporous network structure and a relatively large ratio. surface area, and macroporous adsorption resins are more and more used in the purification and separation of active ingredients and effective parts of traditional Chinese medicines and natural medicines, and the macroporous adsorption resins can be regenerated and reused, and the production cost is low, providing A method for extracting refined gypenoside from Gynostemma pentaphyllum, is characterized in that: comprises the steps:
（1）取绞股蓝全草，粉碎成粗粉或切成小段，加较高浓度醇，回流提取1-3次，每次0.5-3小时，滤过，滤液回收醇，加水溶解，滤过，得滤液；(1) Take the whole Gynostemma pentaphylla, crush it into coarse powder or cut it into small pieces, add higher concentration alcohol, reflux extraction 1-3 times, 0.5-3 hours each time, filter, recover alcohol from the filtrate, add water to dissolve, filter, get the filtrate;
（2）将滤液上于大孔吸附树脂柱上，使绞股蓝中的有效成分缓慢吸附于柱床内的树脂上，以水洗脱，再用较低浓度碱液洗脱除杂，再用水洗至中性，洗脱液弃去；(2) Put the filtrate on the macroporous adsorption resin column, so that the active ingredients in Gynostemma pentaphyllum are slowly adsorbed on the resin in the column bed, eluted with water, then eluted with a lower concentration of lye to remove impurities, and then washed with water To neutrality, the eluent was discarded;
（3）再用较低浓度醇洗脱以适合的流速除杂，低浓度乙醇洗液弃去；(3) Elute with a lower concentration of alcohol to remove impurities at a suitable flow rate, and discard the low concentration ethanol washing solution;
（4）再用较高浓度醇以适合的流速洗脱绞股蓝总皂苷，收集较高浓度醇洗脱液，合并，回收，再减压干燥，即为绞股蓝总皂苷。(4) Elute Gypenosides with a higher concentration of alcohol at a suitable flow rate, collect the eluate from a higher concentration of alcohol, combine, recover, and dry under reduced pressure to obtain Gypenosides.
本发明中采用紫外分光光度法测定制得的绞股蓝总皂中的总皂苷含量，以绞股蓝皂苷A计，含量为92%~94%。In the present invention, the total saponin content in the prepared Gynostemma pentaphylla total soap is measured by ultraviolet spectrophotometry, and the content is 92% to 94% in terms of Gypenoside A.
进一步地，所述步骤(1)的较高浓度醇为40%-95%的甲醇或乙醇，所用量为药材量的6-30倍；Further, the higher concentration of alcohol in the step (1) is 40%-95% methanol or ethanol, and the amount used is 6-30 times the amount of medicinal materials;
进一步地，所述步骤(2)所述的较低浓度碱液为0.5%-10%的氢氧化钠或氢氧化钾或氨试液，洗脱剂用量为树脂体积的1-7倍；Further, the lower concentration alkali solution described in the step (2) is 0.5%-10% sodium hydroxide or potassium hydroxide or ammonia test solution, and the amount of eluent is 1-7 times of the volume of the resin;
进一步地，所述步骤(1)中，所述的绞股蓝全草为切成短段的绞股蓝或者粉碎成粗粉的绞股蓝；Further, in the step (1), the whole herb of Gynostemma pentaphyllum is Gynostemma pentaphyllum cut into short sections or Gynostemma pentaphyllum pulverized into coarse powder;
进一步地，所述步骤(2)中，所述的绞股蓝中的有效成分为绞股蓝皂苷；Further, in the step (2), the active ingredient in the described Gynostemma pentaphyllum is Gypenoside;
进一步地，所述步骤(2)中，所用的大孔树脂为弱极性和非极性大孔吸附树脂，包括但不限于AB-8，D101，HPD100，NKA-2等；Further, in the step (2), the macroporous resins used are weakly polar and nonpolar macroporous adsorption resins, including but not limited to AB-8, D101, HPD100, NKA-2, etc.;
进一步地，所述步骤(3)的较低浓度醇为20%-40%的甲醇或乙醇，流速为0.5-2倍柱体积每小时，洗脱剂用量为树脂体积的2-6倍；Further, the lower concentration of alcohol in the step (3) is 20%-40% methanol or ethanol, the flow rate is 0.5-2 times the column volume per hour, and the amount of eluent is 2-6 times the volume of the resin;
进一步地，所述步骤(4)的较高浓度醇为50%-95%的甲醇或乙醇，流速为0.5-2倍柱体积每小时，洗脱剂用量为树脂体积的2-8倍。Further, the higher concentration alcohol in the step (4) is 50%-95% methanol or ethanol, the flow rate is 0.5-2 times column volume per hour, and the amount of eluent is 2-8 times the volume of the resin.
与现有技术相比，本发明的优点在于，Compared with the prior art, the present invention has the advantage that,
本方法中仅应用一次树脂纯化，不采用正丁醇萃取，即达到纯化效果，其损失的皂苷量少，成本低，周期短。本发明的从绞股蓝中提取纯化绞股蓝总皂苷的方法，可用于工业化生产，成本低，工艺流程短。In this method, resin purification is only applied once, and n-butanol extraction is not used, and the purification effect is achieved, the amount of saponin lost is small, the cost is low, and the cycle is short. The method for extracting and purifying total saponins of Gynostemma pentaphyllum from Gynostemma pentaphyllum of the present invention can be used in industrialized production, has low cost and short process flow.
附图说明Description of drawings
图1是紫外分光光度法测定总皂苷含量图。Fig. 1 is the figure of measuring total saponin content by ultraviolet spectrophotometry.
具体实施方式detailed description
实施例1Example 1
取绞股蓝全草1500克，切成短断，加70%乙醇20倍量，回流提取3小时，滤过，滤液加收乙醇至尽，加水7500mL，煮沸30分钟，滤过，将滤液上于AB-8柱（已处理，Vol=1500mL），5小时上样完毕，流出液弃去；以水洗2BV，水洗液弃去；再用0.2%氢氧化钠洗2BV（3000mL），碱洗液弃去（除掉黄酮类物质），1BV/h；再用水洗至中性（约6BV），水洗液弃去，2BV/h；然后用40%乙醇4BV（6000mL）洗脱，1BV/h ，40%乙醇洗液弃去；再用80%乙醇4BV（6000mL）洗脱，1BV/h，收集80%乙醇洗液，回收乙醇，浓缩成稠膏，再减压干燥，即得绞股蓝总皂苷；采用紫外分光光度法测定总皂苷含量，以绞股蓝皂苷A计，含量为92%。Take 1500 grams of Gynostemma pentaphylla, cut into short pieces, add 20 times the amount of 70% ethanol, reflux extraction for 3 hours, filter, add ethanol to the filtrate to the end, add water 7500mL, boil for 30 minutes, filter, put the filtrate on AB -8 column (processed, Vol=1500mL), after 5 hours of sample loading, discard the effluent; wash 2BV with water, discard the washing solution; then wash 2BV (3000mL) with 0.2% sodium hydroxide, discard the alkali washing solution (to remove flavonoids), 1BV/h; then wash with water until neutral (about 6BV), discard the washing solution, 2BV/h; then elute with 40% ethanol 4BV (6000mL), 1BV/h, 40% Discard the ethanol lotion; then elute with 80% ethanol 4BV (6000mL), 1BV/h, collect the 80% ethanol lotion, recover the ethanol, concentrate into a thick paste, and then dry under reduced pressure to obtain the total saponins of Gynostemma pentaphyllum; The total saponin content was determined by spectrophotometry, and the content was 92% based on Gypenoside A.
实施例2Example 2
取绞股蓝全草3000克，粉碎成粗粉，加85%甲醇15倍量，回流提取2小时，滤过，滤液加收甲醇至尽，加水20L，煮沸30分钟，滤过，将滤液上于D101柱（已处理，Vol=3000mL），6小时上样完毕，流出液弃去；以水洗3BV，水洗液弃去；再用0.5%氢氧化钾洗2BV（6000mL），碱洗液弃去，1.5BV/h；再用水洗至中性（约6BV），水洗液弃去，2BV/h；然后用30%甲醇4BV（6000mL）洗脱，1BV/h ，30%甲醇洗液弃去；再用70%甲醇5BV洗脱，1BV/h，收集70%甲醇洗液，回收甲醇，浓缩成稠膏，再减压干燥，即为绞股蓝总皂苷；采用紫外分光光度法测定总皂苷含量，以绞股蓝皂苷A计，含量为94%。Take 3000 grams of Gynostemma pentaphyllum, crush it into coarse powder, add 15 times the amount of 85% methanol, reflux for extraction for 2 hours, filter, add methanol to the filtrate to the end, add 20L of water, boil for 30 minutes, filter, and put the filtrate on D101 Column (processed, Vol=3000mL), sample loading was completed in 6 hours, and the effluent was discarded; 3BV was washed with water, and the water wash was discarded; then 2BV (6000mL) was washed with 0.5% potassium hydroxide, and the alkali wash was discarded, 1.5 BV/h; then wash with water until neutral (about 6BV), discard the washing solution, 2BV/h; then elute with 30% methanol 4BV (6000mL), 1BV/h, discard the 30% methanol washing solution; 70% methanol 5BV elution, 1BV/h, collect 70% methanol lotion, recover methanol, concentrate into a thick paste, and then dry under reduced pressure, which is the total saponins of Gypenoside; In terms of A, the content is 94%.
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Application publication date: 20170905 |