CN111214498A - Preparation method of effective components in Huperzia serrata - Google Patents

Preparation method of effective components in Huperzia serrata Download PDF

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Publication number
CN111214498A
CN111214498A CN201811413773.7A CN201811413773A CN111214498A CN 111214498 A CN111214498 A CN 111214498A CN 201811413773 A CN201811413773 A CN 201811413773A CN 111214498 A CN111214498 A CN 111214498A
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extracting
chloroform
huperzia serrata
preparation
parts
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不公告发明人
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Qidong Xingteng Trade Co Ltd
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Qidong Xingteng Trade Co Ltd
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Priority to CN201811413773.7A priority Critical patent/CN111214498A/en
Publication of CN111214498A publication Critical patent/CN111214498A/en
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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
    • A61K36/11—Pteridophyta or Filicophyta (ferns)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • 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
    • A61K2236/33—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
    • 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
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • 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
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • 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
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • 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)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicinal Chemistry (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • General Chemical & Material Sciences (AREA)
  • Rheumatology (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Pain & Pain Management (AREA)

Abstract

The invention discloses a preparation method of effective components in huperzia serrata, which comprises the following steps: pulverizing Huperzia serrata, placing in a paper tube, soaking in ethanol for 23-25 hr, reflux extracting until Dragendorffor's reaction is negative, vacuum concentrating at 55-65 deg.C, dissolving with 0.5mol/LHCl, filtering, extracting with chloroform, adjusting pH of acid water layer to 9.4-9.6, extracting with chloroform for 4-6 times, and extracting with anhydrous Na2SO4Drying, recovering solvent, separating by silica gel column chromatography, sequentially eluting with chloroform-methanol at volume ratio of 48:1, 27:1, 14:1, and 5:1, collecting 14:1 eluate, and concentrating. The preparation method provided by the invention can effectively obtain the effective components in huperzia serrata, has various pharmacological activities of analgesia and anti-inflammation, and can be used as the effective parts of huperzia serrata to be applied to medicine preparation.

Description

Preparation method of effective components in Huperzia serrata
Technical Field
The invention relates to a preparation method of effective components in huperzia serrata.
Background
Huperzia serrata (Thunb.) TrevHuperzia serrata(thunb. ex Murray) trev, also known as serpentine pine. Is perennial herb of huperziaceae, has upright or oblique stem, height of 10-30 cm, diameter of 1.5-3.5 mm in the middle, width of 1.5-4.0 cm in branch and leaf, 2-4 branches, and spore is usually on the upper part of the branch. The leaves are spirally arranged, are sparse, flat and elongated, are narrow and elliptical, are obviously narrowed and straight towards the base, are 1-3 cm long and 1-8 mm wide, are wedge-shaped at the base, extend downwards to form a handle, the tip is sharp or tapered, the edge is straight and does not wrinkle, thick or slightly small and irregular sharp teeth are arranged, the two sides are smooth and glossy, the middle pulse is obvious in protrusion, and the leather is thin. The sporophyll and the sterile leaf are isomorphic; the sporangia grows in the axillary lobe of the sporophyll, with the two ends exposed, kidney-shaped, and yellow. Growing on the wetland under the shade, under the brush, beside the road or on the valley stone with the altitude of 300-2700 m.
Distributed around the world. The whole herb is used as the medicine, is recorded in famous plant drawings and examinations, has the advantages of mild nature, bitter, pungent and slightly sweet taste, has the efficacies of stopping bleeding, dissipating blood stasis, reducing swelling, relieving pain, clearing heat, removing dampness, detoxifying and the like, and is mainly used for treating traumatic injury, internal injury hematemesis, hematuria, hemorrhoid bleeding, leucorrhea, toxic swelling, dental ulcer, scald, fire injury and the like. In recent years, the alkaloid huperzine A (HupA) at the phenolic part of the huperzine A has strong cholinesterase resisting effect, the inhibitory activity of the acetylcholinesterase of the huperzine A is 3 times that of physostigmine, and clinical application proves that the huperzine A tablet has obvious curative effect on treating myasthenia gravis and presenile dementia. However, it is toxic and can cause dizziness, nausea and vomiting when intoxication.
Disclosure of Invention
The invention aims to provide a preparation method of effective components in huperzia serrata.
The invention is realized by the following technical scheme:
a method for preparing effective components from Huperzia serrata comprises the following steps: pulverizing Huperzia serrata, placing 10-20 parts of dry powder in a paper tube, soaking with 75-85 parts of 85-95% ethanol for 23-25h, reflux extracting until Dragendorf's reaction is negative, vacuum concentrating at 55-65 deg.C, dissolving with 0.5mol/LHCl, filtering, extracting with chloroform, adjusting pH of acid water layer to 9.4-9.6, extracting with chloroform for 4-6 times, and extracting with anhydrous Na2SO4Drying, recovering solvent, separating by silica gel column chromatography, sequentially eluting with chloroform-methanol at volume ratio of 48:1, 27:1, 14:1, and 5:1, collecting 14:1 eluate, and concentrating; the raw materials are in parts by weight.
Preferably, in the preparation method, 80 parts of ethanol with the volume fraction of 85-95% is used for soaking for 23-25 h.
Preferably, in the preparation method, the concentration is carried out in vacuum at 55-65 ℃.
Preferably, in the preparation method, the pH of the acid water layer is adjusted to 9.4-9.6.
The invention has the technical effects that:
the preparation method provided by the invention can effectively obtain the effective components in huperzia serrata, has various pharmacological activities of analgesia and anti-inflammation, and can be used as the effective parts of huperzia serrata to be applied to medicine preparation.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
A method for preparing effective components from Huperzia serrata comprises the following steps: pulverizing Huperzia serrata, placing 15 parts of dry powder in a paper tube, soaking in 80 parts of 90% ethanol for 24h, reflux-extracting until Dragendorffor's reaction is negative, vacuum-concentrating at 60 deg.C, dissolving with 0.5mol/LHCl, filtering, extracting with chloroform, adjusting pH of acid water layer to 9.5, extracting with chloroform for 5 times, and extracting with anhydrous Na2SO4Drying, recovering solvent, separating by silica gel column chromatography, sequentially eluting with chloroform-methanol at volume ratio of 48:1, 27:1, 14:1, and 5:1, collecting 14:1 eluate, and concentrating; the raw materials are in parts by weight.
Example 2
A method for preparing effective components from Huperzia serrata comprises the following steps: pulverizing Huperzia serrata, placing 10 parts of dry powder in a paper tube, soaking with 75 parts of 85% ethanol by volume for 23h, reflux-extracting until Dragendorf's reaction is negative, vacuum-concentrating at 55 deg.C, dissolving with 0.5mol/LHCl, filtering, extracting with chloroform, adjusting pH of acid water layer to 9.4, extracting with chloroform for 4 times, and extracting with anhydrous Na2SO4Drying, recovering solvent, separating by silica gel column chromatography, sequentially eluting with chloroform-methanol at volume ratio of 48:1, 27:1, 14:1, and 5:1, collecting 14:1 eluate, and concentrating; the raw materials are in parts by weight.
Example 3
A method for preparing effective components from Huperzia serrata comprises the following steps: pulverizing Huperzia serrata, placing 20 parts of dry powder in a paper tube, soaking in 85 parts of 95% ethanol for 25h, reflux-extracting until Dragendorffor's reaction is negative, vacuum-concentrating at 65 deg.C, dissolving in 0.5mol/LHCl, filtering, extracting with chloroform, adjusting pH of acid water layer to 9.6, extracting with chloroform for 6 times, and extracting with anhydrous Na2SO4Drying, recovering solvent, separating by silica gel column chromatography, sequentially eluting with chloroform-methanol at volume ratio of 48:1, 27:1, 14:1, and 5:1, collecting 14:1 eluate, and concentrating; the raw materials are in parts by weight.
The preparation method provided by the invention can effectively obtain the effective components in huperzia serrata, has various pharmacological activities of analgesia and anti-inflammation, and can be used as the effective parts of huperzia serrata to be applied to medicine preparation.

Claims (4)

1. A preparation method of effective components in Huperzia serrata is characterized by comprising the following steps: pulverizing Huperzia serrata, placing 10-20 parts of dry powder in a paper tube, soaking with 75-85 parts of 85-95% ethanol for 23-25h, reflux extracting until Dragendorf's reaction is negative, vacuum concentrating at 55-65 deg.C, dissolving with 0.5mol/LHCl, filtering, extracting with chloroform, adjusting pH of acid water layer to 9.4-9.6, extracting with chloroform for 4-6 times, and extracting with anhydrous Na2SO4Drying, recovering solvent, separating by silica gel column chromatography, sequentially eluting with chloroform-methanol at volume ratio of 48:1, 27:1, 14:1, and 5:1, collecting 14:1 eluate, and concentrating; the raw materials are in parts by weight.
2. The method of claim 1, wherein: soaking the mixture for 23 to 25 hours by using 80 parts of ethanol with the volume fraction of 85 to 95 percent.
3. The method of claim 1, wherein: vacuum concentrating at 55-65 deg.C.
4. The method of claim 1, wherein: adjusting pH of the acid water layer to 9.4-9.6.
CN201811413773.7A 2018-11-26 2018-11-26 Preparation method of effective components in Huperzia serrata Pending CN111214498A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811413773.7A CN111214498A (en) 2018-11-26 2018-11-26 Preparation method of effective components in Huperzia serrata

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811413773.7A CN111214498A (en) 2018-11-26 2018-11-26 Preparation method of effective components in Huperzia serrata

Publications (1)

Publication Number Publication Date
CN111214498A true CN111214498A (en) 2020-06-02

Family

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Application Number Title Priority Date Filing Date
CN201811413773.7A Pending CN111214498A (en) 2018-11-26 2018-11-26 Preparation method of effective components in Huperzia serrata

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Application publication date: 20200602