CN108743629A - The preparation method of lignans constituents in a kind of lepidogrammitis drymoglossoides Ching - Google Patents

The preparation method of lignans constituents in a kind of lepidogrammitis drymoglossoides Ching Download PDF

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Publication number
CN108743629A
CN108743629A CN201810821726.XA CN201810821726A CN108743629A CN 108743629 A CN108743629 A CN 108743629A CN 201810821726 A CN201810821726 A CN 201810821726A CN 108743629 A CN108743629 A CN 108743629A
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preparation
elution
medicinal extract
lepidogrammitis drymoglossoides
ching
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不公告发明人
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Qidong Chuang Lu New Material Co Ltd
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Qidong Chuang Lu New Material Co Ltd
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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
    • A61K36/11Pteridophyta or Filicophyta (ferns)
    • A61K36/12Filicopsida or Pteridopsida
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04Antibacterial agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/12Antivirals
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00General protective or antinoxious agents
    • A61P39/06Free radical scavengers or antioxidants
    • 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
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • 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)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
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  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of preparation methods of lignans constituents in lepidogrammitis drymoglossoides Ching, and steps are as follows:By lepidogrammitis drymoglossoides Ching pulverizing medicinal materials, 40 mesh sieve is crossed, dry 23-25h, carries out ultrasonic extraction at 55-65 DEG C after being 65-75% alcohol solution dippings 47-49h with volume fraction, extracts 2-4 times, each 40-50min, and filtering merges extracting solution, is concentrated under reduced pressure to give medicinal extract;, through large pore resin absorption column, water, ethanol gradient elution will be used successively, collect 70% alcohol elution, then detach through silica gel column chromatography, use volume ratio 90 successively after the appropriate water dissolution of medicinal extract:1,75:1,45:1,26:1,14:1,5:1 chloroform-methanol elution, collects 14:1 elution fraction, concentrates to obtain the final product.Method provided by the invention can quickly obtain lignans constituents in lepidogrammitis drymoglossoides Ching, which has antibacterial, antiviral, antioxidant activity, can be used for drug preparation.

Description

The preparation method of lignans constituents in a kind of lepidogrammitis drymoglossoides Ching
Technical field
The present invention relates to a kind of preparation methods of lignans constituents in lepidogrammitis drymoglossoides Ching.
Background technology
Lepidogrammitis drymoglossoides Ching [Lepidogrammitis drymoglossoides (Baker) Ching, Polypodiaceae] For the herb of fern Polypodiaceae dominoes Cyclosorus plant, root-like stock it is elongated it is horizontal walk, be drilled shape brown lanceolar scale with teeth.Spore Telium is round, respectively in a row along master pulse both sides, between master pulse and limb.Ye Yuansheng, at a distance of 1.5-5 centimetres, two types;No Leaf oblong is educated to oval, and long 1-2 centimetres or slightly long, round end or blunt circle head, base portion wedge shape, there are few handle, full edges;Fertile frond ligule Or lanceolar, 3-6 centimetres long, wide not as good as 1 centimetre, base portion pinch, there are few handle or tool short handles, sometimes with sterile frond similar shape, meat Matter, do after keratin, above it is smooth, below dredge by scale.
Be distributed widely in the provinces such as China Yangtze river basin and Guizhou, Guangdong, Guangxi, include flavones, alkaloid, sterol, Amino acid and sugared isoreactivity ingredient.With all herbal medicine, there is the effect of clearing heat and detoxicating, dampness removing dispersing blood stasis, be used for sore-throat, lung heat cough Blood, rheumatic arthritis, lymphnoditis, cholecystitis, urolithiasis, traumatic injury, serious case of furuncle carbuncle swells.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of lignans constituents in lepidogrammitis drymoglossoides Ching.
The present invention is realized by following technical solution:
The preparation method of lignans constituents, includes the following steps in a kind of lepidogrammitis drymoglossoides Ching:By lepidogrammitis drymoglossoides Ching pulverizing medicinal materials, 40 mesh are crossed Sieve, dry 23-25h, ultrasonic extraction is carried out after being 65-75% alcohol solution dippings 47-49h with volume fraction at 55-65 DEG C, Extraction 2-4 times, each 40-50min, filtering merge extracting solution, are concentrated under reduced pressure to give medicinal extract;After the appropriate water dissolution of medicinal extract Through large pore resin absorption column, successively with water, 20%, 40%, 60%, 70%, 80%, 95% ethanol gradient elution, collects 70% ethyl alcohol and wash De- position, then detached through silica gel column chromatography, volume ratio 90 is used successively:1,75:1,45:1,26:1,14:1,5:1 chloroform-methanol Elution collects 14:1 elution fraction, concentrates to obtain the final product.
Preferably, it in the preparation method, is dried for 24 hours at 60 DEG C.
Preferably, it is 70% alcohol solution dipping 48h with volume fraction in the preparation method.
Preferably, it in the preparation method, extracts 3 times.
Preferably, in the preparation method, 45min is extracted every time.
Preferably, in the preparation method, 1kg lepidogrammitis drymoglossoides Chings are extracted using 11-13L solvents.
Preferably, in the preparation method, by medicinal extract first to use cotton filtering to be inhaled again with macropore after appropriate water dissolution Attached resin column chromatography separation.
Preferably, in the preparation method, the 6-10mL water dissolutions of 1g medicinal extract.
Preferably, in the preparation method, the large pore resin absorption column is D101 types.
The technology of the present invention effect:
Method provided by the invention can quickly obtain lignans constituents in lepidogrammitis drymoglossoides Ching, which has antibacterial, antiviral, anti- Oxidation activity can be used for drug preparation.
Specific implementation mode
The essentiality content of the present invention is specifically introduced with reference to embodiment.
Embodiment 1
The preparation method of lignans constituents, includes the following steps in a kind of lepidogrammitis drymoglossoides Ching:By lepidogrammitis drymoglossoides Ching pulverizing medicinal materials, 40 mesh are crossed Sieve, it is dry at 60 DEG C that ultrasonic extraction is carried out after being 70% alcohol solution dipping 48h with volume fraction for 24 hours, extract 3 times, every time 45min, filtering merge extracting solution, are concentrated under reduced pressure to give medicinal extract;By medicinal extract first to use cotton filtering to use again after appropriate water dissolution D101 type large pore resin absorption column chromatographic isolations, successively use water, 20%, 40%, 60%, 70%, 80%, 95% ethanol gradient elution, 70% alcohol elution is collected, then is detached through silica gel column chromatography, uses volume ratio 90 successively:1,75:1,45:1,26:1,14:1, 5:1 chloroform-methanol elution, collects 14:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg lepidogrammitis drymoglossoides Chings are extracted using 12L solvents, the 8mL water dissolutions of 1g medicinal extract.
Embodiment 2
The preparation method of lignans constituents, includes the following steps in a kind of lepidogrammitis drymoglossoides Ching:By lepidogrammitis drymoglossoides Ching pulverizing medicinal materials, 40 mesh are crossed Sieve, the dry 23h at 55 DEG C, carries out ultrasonic extraction after being 65% alcohol solution dipping 47h with volume fraction, extract 2 times, every time 40min, filtering merge extracting solution, are concentrated under reduced pressure to give medicinal extract;By medicinal extract first to use cotton filtering to use again after appropriate water dissolution D101 type large pore resin absorption column chromatographic isolations, successively use water, 20%, 40%, 60%, 70%, 80%, 95% ethanol gradient elution, 70% alcohol elution is collected, then is detached through silica gel column chromatography, uses volume ratio 90 successively:1,75:1,45:1,26:1,14:1, 5:1 chloroform-methanol elution, collects 14:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg lepidogrammitis drymoglossoides Chings are extracted using 11L solvents, the 6mL water dissolutions of 1g medicinal extract.
Embodiment 3
The preparation method of lignans constituents, includes the following steps in a kind of lepidogrammitis drymoglossoides Ching:By lepidogrammitis drymoglossoides Ching pulverizing medicinal materials, 40 mesh are crossed Sieve, the dry 25h at 65 DEG C, carries out ultrasonic extraction after being 75% alcohol solution dipping 49h with volume fraction, extract 4 times, every time 50min, filtering merge extracting solution, are concentrated under reduced pressure to give medicinal extract;By medicinal extract first to use cotton filtering to use again after appropriate water dissolution D101 type large pore resin absorption column chromatographic isolations, successively use water, 20%, 40%, 60%, 70%, 80%, 95% ethanol gradient elution, 70% alcohol elution is collected, then is detached through silica gel column chromatography, uses volume ratio 90 successively:1,75:1,45:1,26:1,14:1, 5:1 chloroform-methanol elution, collects 14:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg lepidogrammitis drymoglossoides Chings are extracted using 13L solvents, the 10mL water dissolutions of 1g medicinal extract.
Method provided by the invention can quickly obtain lignans constituents in lepidogrammitis drymoglossoides Ching, which has antibacterial, disease-resistant Poison, antioxidant activity can be used for drug preparation.

Claims (9)

1. the preparation method of lignans constituents in a kind of lepidogrammitis drymoglossoides Ching, it is characterised in that include the following steps:By lepidogrammitis drymoglossoides Ching medicinal material It crushes, crosses 40 mesh sieve, the dry 23-25h at 55-65 DEG C, after being 65-75% alcohol solution dippings 47-49h with volume fraction Ultrasonic extraction is carried out, is extracted 2-4 times, each 40-50min, filtering merges extracting solution, is concentrated under reduced pressure to give medicinal extract;Medicinal extract is used Through large pore resin absorption column after appropriate water dissolution, use successively water, 20%, 40%, 60%, 70%, 80%, 95% ethanol gradient elution, 70% alcohol elution is collected, then is detached through silica gel column chromatography, uses volume ratio 90 successively:1,75:1,45:1,26:1,14:1, 5:1 chloroform-methanol elution, collects 14:1 elution fraction, concentrates to obtain the final product.
2. preparation method according to claim 1, it is characterised in that:It is dried for 24 hours at 60 DEG C.
3. preparation method according to claim 1, it is characterised in that:It is 70% alcohol solution dipping 48h with volume fraction.
4. preparation method according to claim 1, it is characterised in that:Extraction 3 times.
5. preparation method according to claim 4, it is characterised in that:Extraction 45min every time.
6. preparation method according to claim 1, it is characterised in that:1kg lepidogrammitis drymoglossoides Chings are extracted using 11-13L solvents.
7. preparation method according to claim 1, it is characterised in that:By medicinal extract first to use cotton mistake after appropriate water dissolution Large pore resin absorption column chromatographic isolation is used in filter again.
8. preparation method according to claim 7, it is characterised in that:The 6-10mL water dissolutions of 1g medicinal extract.
9. preparation method according to claim 7, it is characterised in that:The large pore resin absorption column is D101 types.
CN201810821726.XA 2018-07-24 2018-07-24 The preparation method of lignans constituents in a kind of lepidogrammitis drymoglossoides Ching Withdrawn CN108743629A (en)

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CN201810821726.XA CN108743629A (en) 2018-07-24 2018-07-24 The preparation method of lignans constituents in a kind of lepidogrammitis drymoglossoides Ching

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Application publication date: 20181106