CN107126452A - Gypenosides and preparation method thereof - Google Patents

Gypenosides and preparation method thereof Download PDF

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Publication number
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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gypenosides
alcohol
preparation
resin
ethanol
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胡义扬
冯琴
彭景华
田华捷
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Shuguang Hospital Affiliated to Shanghai University of TCM
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Shuguang Hospital Affiliated to Shanghai University of TCM
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/42Cucurbitaceae (Cucumber family)
    • A61K36/424Gynostemma
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to a kind of gypenosides and preparation method thereof.Belong to the field of Chinese medicines, be related to effective ingredient in Chinese and its extraction, purifying and process for purification, refer specifically to one kind Hydrolysis kinetics gypenoside and preparation method thereof from gynostemma pentaphyllum herb raw material.Gynostemma pentaphyllum is placed in refluxing extraction device by the present invention carries out refluxing extraction with high concentration ethanol, filtration, except alcohol is obtained without alcohol filtrate, filtrate carries out absorb-elute with macroreticular resin, eluent is respectively water, low concentration alkali, low concentration alcohol and high concentration alcohol, after progressively eluting, obtain each eluent, retain high concentration alcohol eluen, concentration is evaporated, and produces gypenosides.Obtained gynostemma pentaphyllum total soap uses determined by ultraviolet spectrophotometry total saponin content therein in terms of gypenoside A, and content is 92% ~ 94%.The inventive method efficiency high, step simplifies, and the cycle is short, and cost is low, it is adaptable to industrialized production.

Description

Gypenosides and preparation method thereof
Technical field
The invention belongs to the field of Chinese medicines, be related to effective ingredient in Chinese and its extraction, purifying and process for purification, refer specifically to it is a kind of from Hydrolysis kinetics gypenoside and preparation method thereof in gynostemma pentaphyllum herb raw material.
Background technology
Prior art discloses gynostemma pentaphylla herbaceous plant, also known as seven leaf courages, five are climbed up by holding on to for Curcurbitaceae gynostemma pentaphyllum genus are perennial Ye Can, public arched bottom, take root with gynostemma pentaphyllum makino etc., Latin literary fame is Gynostemmapentaphyllum (Thunb.) Makino.The plant is divided into 13 kinds, is distributed in China, Japan and Korea and Southeast Asian countries, wherein, show according to investigations, There are 11 kinds of presence in China, i.e.,:Single leaf gynostemma pentaphyllum, G. laxum, Burma gynostemma pentaphylla, hair gynostemma pentaphylla, longstipe gynostemma herb, peck fruit Gynostemma pentaphylla, heart seed gynostemma pentaphylla, small seed gynostemma pentaphylla, poly- fruit gynostemma pentaphylla, flower thinning gynostemma pentaphylla;Its bitter, property are sweet cold, nontoxic, with clear Thermal detoxification, tonifying Qi promote the production of body fluid, expelling phlegm and arresting coughing, the effect for controlling nocturnal emission with astringent drugs of calming the nerves, cure mainly chronic bronchitis, cough, asthma, infectiousness liver The diseases such as inflammation, pyelonephritis, and forgetful insomnia, burnout are eaten less, emission.
Contain saponins material, Flavonoid substances, polysaccharose substance, vitamins thing in studies have shown that gynostemma pentaphylla plant The active ingredients such as matter, mushroom class class material, organic acid substance, alkaloids substance, protein substance.Saponins material is it One of main component, gypenoside contains ginsenoside identical tetracyclic triterpene dammarane type structure.Saponin(e contains in gynostemma pentaphylla Measure and relatively enrich, the priority separation from gynostemma pentaphylla of relevant research at present identifies more than 80 and plants saponin(e.Studies have shown that gynostemma pentaphylla Saponin(e has reducing blood lipid, norcholesterol, hypotensive, enhancing coronary artery and cerebral blood flow (CBF), anti-DNA variation effect, raising machine Body immunity function etc. is acted on.
At present, the general extraction methods for saponins material being extracted from Gynostemma pentaphyllum add water to cook method, organic solvent Reflux extraction, percolation etc., and have the various new technologies such as Microwave Extraction, ultrasonic extraction, enzyme assisted extraction;But it is therein Refined method is few, the main characteristic big using saponins material solubility in n-butanol, with extracting n-butyl alcohol, but positive fourth Alcohol boiling point is high, and recovery is not easy, and residual quantity is larger in end-product, and industrialized production is difficult.
Present situation based on prior art, present inventor intends providing a kind of effective ingredient in Chinese and its extraction, purifying And refined method, Hydrolysis kinetics gypenoside and preparation method thereof especially from gynostemma pentaphyllum herb raw material.This method will There is realistic meaning to industrialized production Hydrolysis kinetics gypenoside.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of effective ingredient in Chinese and its extraction, purifying and refined side Method, and in particular to gypenosides and preparation method thereof, especially one kind can industrialized production, cost is low, and technological process is short The method of extraction purification gypenosides from gynostemma pentaphylla.
The present invention solves the technical scheme that is used of above-mentioned technical problem to be that a class is free of exchange base based on macroporous absorbent resin Group and the preparation for having macroporous structure, with good macroreticular structure and larger specific surface area, and, greatly Macroporous adsorbent resin is more and more applied to Chinese medicine and natural drug active ingredient, the purifying of active component and separated, and, it is described Macroporous absorbent resin it is renewable reuse, the characteristics of production cost is low there is provided one kind from gynostemma pentaphylla Hydrolysis kinetics twist The method of the blue saponin(e of stock, it is characterised in that:Comprise the following steps:
(1)Gynostemma pentaphyllum herb is taken, coarse powder is ground into or is cut into segment, plus higher concentration alcohol, refluxing extraction 1-3 times, each 0.5-3 Hour, filtration, filtrate reclaims alcohol, is dissolved in water, and filters, obtains filtrate;
(2)By on filtrate on large pore resin absorption column, make the active ingredient in gynostemma pentaphylla be slowly adsorbed in post bed in resin On, with water elution, then with the elution removal of impurities of low concentration alkali lye, it is washed with water to neutrality, eluent is discarded;
(3)Again with the elution of low concentration alcohol with suitable flow velocity removal of impurities, low-concentration ethanol washing lotion is discarded;
(4)Gypenosides are eluted with suitable flow velocity with higher concentration alcohol again, higher concentration alcohol eluen is collected, merged, Reclaim, then be dried under reduced pressure, as gypenosides.
The total saponin content in gynostemma pentaphyllum total soap made from determined by ultraviolet spectrophotometry is used in the present invention, with gynostemma pentaphylla Saponin A meter, content is 92% ~ 94%.
Further, the higher concentration alcohol of the step (1) is 40%-95% methanol or ethanol, and amount used is medicinal material amount 6-30 times;
Further, the low concentration alkali lye described in the step (2) is 0.5%-10% sodium hydroxide or potassium hydroxide or ammonia Test solution, eluting agent is 1-7 times of resin volume;
Further, in the step (1), described gynostemma pentaphyllum herb is to be cut into the gynostemma pentaphylla of short section or be ground into coarse powder Gynostemma pentaphylla;
Further, in the step (2), the active ingredient in described gynostemma pentaphylla is gypenoside;
Further, in the step (2), macroreticular resin used is low pole and nonpolar macroporous adsorption resin, including but It is not limited to AB-8, D101, HPD100, NKA-2 etc.;
Further, the low concentration alcohol of the step (3) is 20%-40% methanol or ethanol, and flow velocity is 0.5-2 times of column volume Per hour, eluting agent is 2-6 times of resin volume;
Further, the higher concentration alcohol of the step (4) is 50%-95% methanol or ethanol, and flow velocity is 0.5-2 times of column volume Per hour, eluting agent is 2-8 times of resin volume.
Compared with prior art, it is an advantage of the current invention that
Only extracting n-butyl alcohol is not used, that is, reaches purification effect using a purifying resin in this method, its saponin(e amount lost Few, cost is low, and the cycle is short.The method of extraction purification gypenosides from gynostemma pentaphylla of the present invention, available for industrial metaplasia Production, cost is low, and technological process is short.
Brief description of the drawings
Fig. 1 is determined by ultraviolet spectrophotometry total saponin content figure.
Embodiment
Embodiment 1
1500 grams of gynostemma pentaphyllum herb is taken, short disconnected, plus 70% ethanol, 20 times of amounts are cut into, refluxing extraction 3 hours, filtration, filtrate adds second Alcohol to the greatest extent, add water 7500mL, boils 30 minutes, filtration, by filtrate in AB-8 posts(It is processed, Vol=1500mL), on 5 hours Sample is finished, and efflux is discarded;To wash 2BV, water lotion is discarded;Again with 0.2% caustic washing 2BV(3000mL), alkali wash water abandons Go(Remove Flavonoid substances), 1BV/h;It is washed with water to neutrality(About 6BV), water lotion discards, 2BV/h;Then 40% ethanol is used 4BV(6000mL)Elution, 1BV/h, 40% ethanol washing lotion is discarded;Again with 80% ethanol 4BV(6000mL)Elution, 1BV/h is collected 80% ethanol washing lotion, reclaims ethanol, is condensed into thick paste, then is dried under reduced pressure, and produces gypenosides;Using uv-spectrophotometric Method determines total saponin content, and in terms of gypenoside A, content is 92%.
Embodiment 2
3000 grams of gynostemma pentaphyllum herb is taken, coarse powder, plus 85% methanol, 15 times of amounts are ground into, refluxing extraction 2 hours, filtration, filtrate is added Methanol to the greatest extent, add water 20L, boils 30 minutes, filtration, by filtrate in D101 posts(It is processed, Vol=3000mL), on 6 hours Sample is finished, and efflux is discarded;To wash 3BV, water lotion is discarded;Again 2BV is washed with 0.5% potassium hydroxide(6000mL), alkali wash water abandons Go, 1.5BV/h;It is washed with water to neutrality(About 6BV), water lotion discards, 2BV/h;Then with 30% methanol 4BV(6000mL)Wash De-, 1BV/h, 30% methanol washing lotion is discarded;Eluted again with 70% methanol 5BV, 1BV/h, collect 70% methanol washing lotion, reclaim methanol, Thick paste is condensed into, then is dried under reduced pressure, as gypenosides;Using determined by ultraviolet spectrophotometry total saponin content, to twist The blue saponin A meter of stock, content is 94%.

Claims (9)

1. the preparation method of gypenosides, it is characterised in that it includes step:
(1)Gynostemma pentaphyllum herb, plus higher concentration alcohol are taken, refluxing extraction 1-3 times is each 0.5-3 hours, filtered, filtrate reclaims alcohol, It is dissolved in water, filters, obtain filtrate;
(2)By on filtrate on large pore resin absorption column, make the active ingredient in gynostemma pentaphylla be slowly adsorbed in post bed in resin On, with water elution, then with the elution removal of impurities of low concentration alkali lye, it is washed with water to neutrality, eluent is discarded;
(3)Eluted with low concentration alcohol with suitable flow velocity removal of impurities, low-concentration ethanol washing lotion is discarded;
(4)Gypenosides are eluted with suitable flow velocity with higher concentration alcohol, higher concentration alcohol eluen is collected, merges, return Receive, then be dried under reduced pressure, obtain gypenosides.
2. the preparation method of the gypenosides as described in claim 1, it is characterised in that the step(1)In, it is more highly concentrated Methanol or ethanol that alcohol is 40%-95% are spent, consumption is 6-30 times of medicinal material amount.
3. the preparation method of the gypenosides as described in claim 1, it is characterised in that the step(2)In, it is relatively low dense Sodium hydroxide or potassium hydroxide or ammonia solution that alkali lye is 0.5%-10% are spent, eluting agent is 1-7 times of resin volume.
4. the preparation method of the gypenosides as described in claim 1, it is characterised in that the step(3)In, it is relatively low dense Methanol or ethanol that alcohol is 20%-40% are spent, for 0.5-2 times of column volume per hour, eluting agent is the 2-6 of resin volume to flow velocity Times.
5. the preparation method of the gypenosides as described in claim 1, it is characterised in that the step(4)In, it is more highly concentrated Methanol or ethanol that alcohol is 50%-95% are spent, for 0.5-2 times of column volume per hour, eluting agent is the 2-8 of resin volume to flow velocity Times.
6. the preparation method of the gypenosides as described in claim 1, it is characterised in that in described step (1), strand Blue herb is the gynostemma pentaphylla for being cut into short section or the gynostemma pentaphylla for being ground into coarse powder.
7. the preparation method of the gypenosides as described in claim 1, it is characterised in that in described step (2), strand Active ingredient in basket is gypenoside.
8. the preparation method of the gypenosides as described in claim 1, it is characterised in that described step(2)In, it is used Macroreticular resin be low pole and nonpolar macroporous adsorption resin, selected from AB-8, D101, HPD100 or NKA-2.
9. the preparation method of the gypenosides as described in claim 1, it is characterised in that in obtained gypenosides Total saponin content, in terms of gypenoside A, content be 92% ~ 94%.
CN201610106326.1A 2016-02-26 2016-02-26 Gypenosides and preparation method thereof Pending CN107126452A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484711A (en) * 2018-03-23 2018-09-04 娄志春 A method of preparing gypenoside LI
CN108484713A (en) * 2018-03-23 2018-09-04 娄志春 A method of preparing gypenoside L
CN110025650A (en) * 2019-05-31 2019-07-19 嘉应学院医学院 The content assaying method of gypenosides in the preparation method and Herb Gynostemmae Pentaphylli extract of a kind of Herb Gynostemmae Pentaphylli extract
CN111349135A (en) * 2018-12-23 2020-06-30 徐世明 Method for extracting gypenoside XLIX and medicine for treating diabetes and hyperlipidemia
CN112159451A (en) * 2020-09-29 2021-01-01 杨凌萃健生物工程技术有限公司 Gynostemma pentaphylla saponin extract and preparation method thereof

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CN103191188A (en) * 2013-04-01 2013-07-10 上海现代中医药股份有限公司 Six-ingredient botanical composition for treating hepatic fibrosis and preparation method thereof
CN103923149A (en) * 2014-04-15 2014-07-16 厦门华侨亚热带植物引种园 Gynostemma pentaphylla saponin XLV Ed and preparation method thereof

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CN1517358A (en) * 2003-01-16 2004-08-04 北京大学安康药物研究院 Preparation method of gynostemma pentaphylia total saponin
CN103191188A (en) * 2013-04-01 2013-07-10 上海现代中医药股份有限公司 Six-ingredient botanical composition for treating hepatic fibrosis and preparation method thereof
CN103923149A (en) * 2014-04-15 2014-07-16 厦门华侨亚热带植物引种园 Gynostemma pentaphylla saponin XLV Ed and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484711A (en) * 2018-03-23 2018-09-04 娄志春 A method of preparing gypenoside LI
CN108484713A (en) * 2018-03-23 2018-09-04 娄志春 A method of preparing gypenoside L
CN111349135A (en) * 2018-12-23 2020-06-30 徐世明 Method for extracting gypenoside XLIX and medicine for treating diabetes and hyperlipidemia
CN110025650A (en) * 2019-05-31 2019-07-19 嘉应学院医学院 The content assaying method of gypenosides in the preparation method and Herb Gynostemmae Pentaphylli extract of a kind of Herb Gynostemmae Pentaphylli extract
CN112159451A (en) * 2020-09-29 2021-01-01 杨凌萃健生物工程技术有限公司 Gynostemma pentaphylla saponin extract and preparation method thereof

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