CN107661361A - A kind of process for super-critical extracting of ginko leaves flavone class compound - Google Patents

A kind of process for super-critical extracting of ginko leaves flavone class compound Download PDF

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CN107661361A
CN107661361A CN201711144692.7A CN201711144692A CN107661361A CN 107661361 A CN107661361 A CN 107661361A CN 201711144692 A CN201711144692 A CN 201711144692A CN 107661361 A CN107661361 A CN 107661361A
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super
extract
class compound
extraction
liquid
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贾建洪
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Shangyu Research Institute of ZJUT
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Shangyu Research Institute of ZJUT
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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
    • A61K36/16—Ginkgophyta, e.g. Ginkgoaceae (Ginkgo family)
    • 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
    • A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • 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
    • A61K2236/30—Extraction of the material
    • A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
    • 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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  • 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)
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  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
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  • 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 process for super-critical extracting of ginko leaves flavone class compound, raw material is not required to dry and directly used, and power consumption is few, and extract yield is high, and potential safety hazard is low.Fresh ginkgo leaf is handled using enzymatic isolation method in extraction process, clasmatosis is abundant, ensure that extraction efficiency.There is the feature of environmental protection, nonhazardous and noresidue as extractant using supercritical carbon dioxide, beeswax can significantly improve the extraction content of flavones as entrainer.

Description

A kind of process for super-critical extracting of ginko leaves flavone class compound
Technical field
The present invention relates to a kind of extraction process, more particularly to a kind of means of supercritical extraction work of ginko leaves flavone class compound Skill.
Background technology
Ginkgo is exactly our usually said maidenhair trees, is a kind of deciduous tree relatively common in China, it is current One of species most long-lived in the world known to us, nowadays most long-lived ginkgo be located at China Guizhou, its age of tree reaches By 5000 or six thousand years as long as.Ginkgo be before more than 500,000,000 years the Carboniferous Period occur, the appearance of quaternary glacier motion, make the ring of the earth Cold that border becomes suddenly, increasingly be not suitable for most plants existence, this period major part ginkgo class plant all oneself Through disappearing, worldwide just only selected areas of China just survives because of the factor of natural environment.Ginkgo is naked son The existing unique species of plant Ginkgo biloba mouth, and it with mouth its species all oneself disappear in the long korneforos of history, Just because of this, silver Apricot is just referred to as the ＂ living fossils ＂ of plant kingdom.
Proved by present medical research and clinical test, the medical value of ginkgo leaf is very high, central containing largely can be with The medicinal ingredient utilized, these medicinal ingredients share kind about more than 200 according to incompletely statistics, and wherein it is extractable utilize it is medicinal Composition account for about 160 kinds, and yellow Seoul classes active material shares as many as 35 kinds among these medicinal ingredients.These medicinal ingredients Primary efficacy be embodied in anti-inflammatory, beauty, anti-oxidant, anti-aging etc., in addition, the flavone compound in ginkgo leaf also has There is promotion blood circulation of human body, adjust cardiovascular Diastolic Force, reduce the effects such as blood glucose, increase CBF.Huang in ginkgo leaf Beautiful class compound in terms of beauty have whitening, it is crease-resistant the effect of.Yellow Seoul classes compound contained by it can reduce color in human body Element formation and precipitation, part oligo-element can W suppress human body in melanin produce, increase human body myocyte's moral vigor, tool There are whitening and preventing and treating patch.The yellow beautiful constituents in ginkgo leaf can also protect corium confluent monolayer cells simultaneously, improve people's flesh Vitality of subject, promote the circulation of blood in human body in liquid, prevent cell to be oxidized, so as to play the effect of crease-resistant.
Flavone compound in ginkgo leaf as medicinal ingredient oneself through there is the history of decades, and it is main component Medicine product since the advent of the world just sell well and do not wane.Eighties of last century, since Germany scientist has applied for the patent of extraction process earliest Afterwards, the yellow beautiful extracting method of ginkgo leaf is with regard to of great interest, by the development in a nearly century, on yellow in ginkgo leaf The extracting method of ketone compounds can substantially be divided into following several：It is traditional extraction method, ultrasonic extraction, enzyme extraction method, super Critical fluids extraction method, microwave loss mechanisms.
The patent No. 200410069037.6, entitled " a kind of ginkgo biloba p.e and its extracting method, although being carried with ethanol The flavones taken has reached 80%, but the flavones total amount and active component of its extraction, is far from reaching preferable requirement.For existing The deficiency of technology, it is desirable to provide a kind of method for the recovery rate for improving the yellow reward of ginkgo leaf, change and carried in the current ginkgo industry in China Take the present situation that rate is low.
The content of the invention
It is an object of the invention to provide a kind of technique is simple, without using toxic organic solvents, extracted using macroreticular resin The technique of ginko leaves flavone class compound, it is a kind of separation easy to operate, recovery rate is high, is suitable for industrialized production uses Technology.
A kind of process for super-critical extracting of ginko leaves flavone class compound provided by the invention, step include：
1) enzymolysis processing：A certain amount of ethanol is added after fresh ginkgo leaf is crushed, is added after stirring evenly equivalent to ginkgo leaf The pectase of weight 0.1%~0.3% and the hemicellulase equivalent to ginkgo leaf weight 0.9%~1.6%, at 25~40 DEG C Enzymolysis processing for a period of time, obtains digesting mixture；
2) supercritical extract：The enzymolysis mixture is imported in extraction kettle, uses supercritical CO2As extractant, honeybee Wax is 20~40 DEG C in extraction temperature as entrainer, and Fluid pressure is 20~40MPa, under 0.10~0.40ml/min of flow velocity, 1~3h of extraction obtains extract, and extract ethanol absorbs the liquid that is absorbed.
3) macroporous resin enrichment：By macroporous resin column adsorption and enrichment in absorbing liquid, the aperture of big pore resin for 100~ 200 angstroms, specific surface area is 500~800m2/ g, decoction flow control is in 2~5mL/min；
4) elute：First with 2~5BV amount water elutions, then with 1~10BV amounts 70% (V/V) ethanol elution, flow velocity control System starts to collect eluent after 2~5mL/min, 1~2BV of eluent outflow, and eluent is crossed into activated-charcoal column, collects liquid, Obtain ginkgo leaf total flavonoid.
Preferably, the ginkgo leaf described in step 1) is fresh leaf of the moisture content 40~60%, and need not be through any dry Dry process processing.The solid-liquid ratio of ginkgo leaf and ethanol solution is 1:0.5~1:2.Described hemicellulase is that can be planted forming The general name of the various enzymes of polysaccharide (except cellulose and pectin substance) hydrolyzable of thing cell membrane；Pectase is from head mold Extraction, intercellular pectic substance is degraded, cell is separated out of tissue.
In step 2), concrete operations are as follows：Enable overcritical device, CO2Gas is filtered with 20L/h flow Extractor is squeezed into by compressor afterwards, to the 20~40MPa of pressure for reaching setting, extraction temperature by extractor chuck circulation water control Make and stably at 20~40 DEG C.
The extract separation process is：CO2After fluid extraction liquid reaches knockout drum decompression, separated with extract, it is described CO2Gas uses into the compressor cycle, extract is absorbed with ethanol, be absorbed liquid.
In step 3), the macroreticular resin is the macroreticular resins such as AB-8, NKA, X-5, NKA-9, S-8, and before the use Need to be pre-processed.
Advantages of the present invention is as follows：
1st, the present invention changes traditional production technology, and raw material is not required to dry and directly used, and power consumption is few, and flavones yield is high, Potential safety hazard is low.Fresh ginkgo leaf deposit is very abundant, and the cost of raw material is low, and cost of transportation is also low.
2nd, fresh ginkgo leaf is handled using enzymatic isolation method in extraction process, clasmatosis is abundant, ensure that extraction efficiency；Using Supercritical carbon dioxide has the characteristics that the feature of environmental protection, nonhazardous W and noresidue as extractant；Beeswax as entrainer, The extraction content of flavones can be significantly improved；Extract is first crossed into resin column, then refined with charcoal absorption, obtained Huang Ketone content is high.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment Only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area The every other embodiment that art personnel are obtained on the premise of creative work is not made, belong to the model that the present invention protects Enclose.
【Embodiment 1】
1) enzymolysis processing：A certain amount of ethanol is added after fresh ginkgo leaf is crushed, is added after stirring evenly equivalent to ginkgo leaf The pectase of weight 0.1% and the hemicellulase equivalent to ginkgo leaf weight 0.9%, at 40 DEG C enzymolysis processing for a period of time, Obtain digesting mixture；
2) supercritical extract：The enzymolysis mixture is imported in extraction kettle, enables overcritical device, CO2Gas with 20L/h flow by compressor squeezes into extractor after being filtered, to the pressure 35MPa for reaching setting, extraction temperature by The circulation water management of extractor chuck and stably at 35 DEG C, while beeswax is imported as entrainer, it is 35 DEG C in extraction temperature, stream Body pressure is 35MPa, and under flow velocity 0.3ml/min, extraction 3h obtains extract, CO2After fluid extraction liquid reaches knockout drum decompression, Separated with extract, the CO2Gas uses into the compressor cycle, extract is absorbed with ethanol, be absorbed liquid.
3) macroporous resin enrichment：By AB-8 macroporous resin columns adsorption and enrichment in absorbing liquid, the aperture of big pore resin is 100 angstroms, specific surface area 600m2/ g, decoction flow control is in 3mL/min.
4) elute：First with 3BV amount water elutions, then existed with 6BV amounts 70% (V/V) ethanol elution, flow control After 3mL/min, eluent outflow 1BV, start to collect eluent, eluent is crossed into activated-charcoal column, liquid is collected, obtains ginkgo leaf General flavone.
【Embodiment 2】
1) enzymolysis processing：A certain amount of ethanol is added after fresh ginkgo leaf is crushed, is added after stirring evenly equivalent to ginkgo leaf The pectase of weight 0.3% and the hemicellulase equivalent to ginkgo leaf weight 1.2%, at 35 DEG C enzymolysis processing for a period of time, Obtain digesting mixture；
2) supercritical extract：The enzymolysis mixture is imported in extraction kettle, enables overcritical device, CO2Gas with 20L/h flow by compressor squeezes into extractor after being filtered, to the pressure 25MPa for reaching setting, extraction temperature by The circulation water management of extractor chuck and stably at 40 DEG C, while beeswax is imported as entrainer, it is 40 DEG C in extraction temperature, stream Body pressure is 25MPa, and under flow velocity 0.4ml/min, extraction 2h obtains extract, CO2After fluid extraction liquid reaches knockout drum decompression, Separated with extract, the CO2Gas uses into the compressor cycle, extract is absorbed with ethanol, be absorbed liquid.
3) macroporous resin enrichment：By the upper NKA macroporous resin column adsorption and enrichments of filtrate, the aperture of big pore resin is 150 Angstrom, specific surface area 700m2/ g, decoction flow control is in 3mL/min.
4) elute：First with 2BV amount water elutions, then existed with 10BV amounts 70% (V/V) ethanol elution, flow control After 3mL/min, eluent outflow 2BV, start to collect eluent, eluent is crossed into activated-charcoal column, liquid is collected, obtains ginkgo leaf General flavone.
【Embodiment 3】
1) enzymolysis processing：A certain amount of ethanol is added after fresh ginkgo leaf is crushed, is added after stirring evenly equivalent to ginkgo leaf The pectase of weight 0.2% and the hemicellulase equivalent to ginkgo leaf weight 1.5%, at 25 DEG C enzymolysis processing for a period of time, Obtain digesting mixture；
2) supercritical extract：The enzymolysis mixture is imported in extraction kettle, enables overcritical device, CO2Gas with 20L/h flow by compressor squeezes into extractor after being filtered, to the pressure 20MPa for reaching setting, extraction temperature by The circulation water management of extractor chuck and stably at 40 DEG C, while beeswax is imported as entrainer, it is 40 DEG C in extraction temperature, stream Body pressure is 20MPa, and under flow velocity 0.2ml/min, extraction 3h obtains extract, CO2After fluid extraction liquid reaches knockout drum decompression, Separated with extract, the CO2Gas uses into the compressor cycle, extract is absorbed with ethanol, be absorbed liquid.
3) macroporous resin enrichment：By the upper S-8 macroporous resin column adsorption and enrichments of filtrate, the aperture of big pore resin is 200 Angstrom, specific surface area 520m2/ g, decoction flow control is in 2mL/min.
4) elute：First with 35BV amount water elutions, then existed with 10BV amounts 70% (V/V) ethanol elution, flow control After 2mL/min, eluent outflow 2BV, start to collect eluent, eluent is crossed into activated-charcoal column, liquid is collected, obtains ginkgo leaf General flavone.
Described above has fully disclosed the embodiment of the present invention.It is pointed out that it is familiar with the field Scope of the technical staff to any change that the embodiment of the present invention is done all without departing from claims of the present invention. Correspondingly, the scope of claim of the invention is also not limited only to previous embodiment.

Claims (6)

1. a kind of process for super-critical extracting of ginko leaves flavone class compound, its step are as follows：
1) enzymolysis processing：A certain amount of ethanol is added after fresh ginkgo leaf is crushed, is added after stirring evenly equivalent to ginkgo leaf weight 0.1%~0.3% pectase and the hemicellulase equivalent to ginkgo leaf weight 0.9%~1.6%, digest at 25~40 DEG C Processing a period of time, obtain digesting mixture；
2) supercritical extract：The enzymolysis mixture is imported in extraction kettle, uses supercritical CO2As extractant, beeswax conduct Entrainer, it is 20~40 DEG C in extraction temperature, Fluid pressure be 20~40MPa, under 0.10~0.40ml/min of flow velocity, extracts 1 ~3h obtains extract, and extract ethanol absorbs the liquid that is absorbed.
3) macroporous resin enrichment：By macroporous resin column adsorption and enrichment in absorbing liquid, the aperture of big pore resin is 100~200 Angstrom, specific surface area is 500~800m2/ g, decoction flow control is in 2~5mL/min；
4) elute：First with 2~5BV amount water elutions, then existed with 1~10BV amounts 70% (V/V) ethanol elution, flow control 2~5mL/min, after eluent flows out 1~2BV, start to collect eluent, eluent is crossed into activated-charcoal column, liquid is collected, obtains Ginkgo leaf total flavonoid.
2. the process for super-critical extracting of ginko leaves flavone class compound according to claim 1, it is characterised in that the silver Apricot leaf is fresh leaf of the moisture content 40~60%, and need not be handled through any drying process.
3. the process for super-critical extracting of ginko leaves flavone class compound is obtained according to claim 1, in the step 1), ginkgo The solid-liquid ratio of leaf and ethanol solution is 1:0.5~1:2.
4. the process for super-critical extracting of ginko leaves flavone class compound according to claim 1, it is characterised in that the step It is rapid 2) in, the extract separation process is：CO2After fluid extraction liquid reaches knockout drum decompression, separated with extract, it is described CO2 gases use into the compressor cycle, extract are absorbed with ethanol, be absorbed liquid.
5. the process for super-critical extracting of ginko leaves flavone class compound according to claim 1, it is characterised in that step 3) In, the macroreticular resin is the macroreticular resins such as AB-8, NKA, X-5, NKA-9, S-8, and needs to be pre-processed before the use.
6. the process for super-critical extracting of the ginko leaves flavone class compound according to any one of Claims 1 to 5, its feature exist In also comprising the following steps in the step 2), enable overcritical device, CO2Gas is filtered with 20L/h flow Extractor is squeezed into by compressor afterwards, to the 20~40MPa of pressure for reaching setting, extraction temperature by extractor chuck circulation water control Make and stably at 20~40 DEG C.
CN201711144692.7A 2017-11-17 2017-11-17 A kind of process for super-critical extracting of ginko leaves flavone class compound Pending CN107661361A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108379316A (en) * 2018-04-18 2018-08-10 佛山市飞程信息技术有限公司 A kind of extracting method of ginsenoside
CN108689873A (en) * 2018-03-27 2018-10-23 佛山市飞程信息技术有限公司 A kind of process for super-critical extracting of capsaicine

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0308675A1 (en) * 1987-09-07 1989-03-29 CHLORINE ENGINEERS CORP., Ltd. Process for the supercritical extraction and separation of solid samples
CN102293791A (en) * 2011-08-18 2011-12-28 湖南麓山天然植物制药有限公司 Production method for extracting effective components of gingko leaf

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0308675A1 (en) * 1987-09-07 1989-03-29 CHLORINE ENGINEERS CORP., Ltd. Process for the supercritical extraction and separation of solid samples
CN102293791A (en) * 2011-08-18 2011-12-28 湖南麓山天然植物制药有限公司 Production method for extracting effective components of gingko leaf

Non-Patent Citations (1)

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蔡锦源等: "银杏黄酮的提取及纯化方法研究进展", 《应用化工》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108689873A (en) * 2018-03-27 2018-10-23 佛山市飞程信息技术有限公司 A kind of process for super-critical extracting of capsaicine
CN108379316A (en) * 2018-04-18 2018-08-10 佛山市飞程信息技术有限公司 A kind of extracting method of ginsenoside

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